Labormahlkörpermühle

Abstract

Laboratory grinding media mill (1), in particular planetary ball mill, centrifugal ball mill or vibrating mill, comprising: a grinding vessel (8) with a grinding bowl (10) and a grinding bowl lid (12) for closing the grinding bowl (10), wherein the grinding vessel (8) defines 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 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 in the laboratory grinding media mill (1), wherein the grinding vessel (8) comprises: at least one sensor (62, 80, 110) which measures a state parameter of the grinding vessel (8) and / or the grinding vessel interior (18), an electronic display device (46) which is arranged on an outer side (9) of the grinding vessel (8) and which displays the state parameter measured by the sensor (62, 80, 110) visibly for the user directly on the outer side of the grinding vessel.

Description

Field of the invention

[0001] The invention relates to a laboratory grinding media mill for process analysis in laboratory applications, in particular a planetary ball mill, a centrifugal ball mill or a vibrating mill on a laboratory scale, in which material to be ground can be finely ground in a closed grinding vessel by permanently changing acceleration in a grinding vessel interior between the grinding media and walls of the grinding vessel by impact and friction effects. Background of the invention

[0002] Laboratory-scale grinding media mills are used, for example, in process analytics for grinding samples. Depending on the sample volume, grinding conditions, and the desired grinding result, e.g., the desired degree of fineness or the quantity of material to be ground, such laboratory-scale grinding media mills can be designed as planetary ball mills, centrifugal ball mills, or vibratory mills, sometimes 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 bottom and / or the annular wall of a cup-like receiving device. Newer planetary mills are, for example,Described 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, and DE 10 2012 009 987 A1. A selection of currently commercially available laboratory-scale planetary mills can also be found on the applicant's website at www.fritsch.de.

[0003] 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 central axis. On the one hand, they orbit the sun axis and on the other hand they rotate about their own axis, the eccentric planetary axis. The rotation and simultaneous rotation of the grinding bowls exerts a changing, radially outward-directed centrifugal force on the material being ground into the grinding bowl. Typically, reusable grinding media, such as grinding balls, are added to the material to be ground; these grind the material with high efficiency through impact and friction between the grinding media and the walls of the grinding vessel. The grinding vessel and grinding media together form the so-called grinding set.

[0004] With certain dimensions of the rotating parts and certain rotational speeds, trajectories can be generated for the material to be ground and the grinding media in a planetary ball mill. The material to be ground and the grinding media then move transversely through the grinding bowl until they hit the inner wall of the grinding bowl. The material to be ground and the grinding media can then be carried along for a short distance along the inner circumference of the grinding bowl until the resulting force again causes the transverse acceleration described above to occur and the material to be ground and the grinding media to perform a flight movement through the grinding bowl. This is also referred to as the "throw mode." When a ball mill operates in the throw mode, a high grinding effect or a high energy input into the material to be ground can be achieved at high speeds.

[0005] In vibratory mills, a grinding vessel consisting of a grinding bowl and a grinding bowl lid is subjected to a permanently changing acceleration, typically in an oscillating or vibrating motion. In some vibratory mills, the grinding vessels are clamped upright on an oscillating plate as a grinding vessel holder. Such vibratory mills typically operate with a single or a few larger grinding media, e.g., ring-shaped or disc-shaped grinding media (grinding discs), which remain in place on the grinding bowl base when the grinding vessel oscillates. An example of a vibratory mill, sometimes also referred to as a disc (vibratory) mill, is the applicant's Pulverisette® 9, cf. www.fritsch.de. However, vibratory mills are also known which may use smaller, typically longitudinally cylindrical grinding vessels with grinding balls, e.g., with a grinding vessel volume of up to 50 ml, where the grinding vessels are mounted horizontally, e.g.are clamped into two horizontally counter-oscillating grinding vessel holders (Boxer principle). The grinding vessels can oscillate back and forth at a defined oscillation frequency, essentially along a straight or slightly curved line, essentially horizontally.

[0006] Laboratory grinding media mills are characterized by fast and effective comminution. They are versatile and ideal for loss-free ultrafine comminution, down to final finenesses in the nanometer range, depending on the mill type. Depending on the application, grinding can be carried out dry, in suspension, or under inert gas. In addition to pure comminution, laboratory grinding media mills can also be used for mixing, alloying, activation, amorphization, or phase transformation processes.

[0007] These processes can involve a relatively high energy input into the material being ground or the grinding vessel, potentially leading to undesirable heating of the material being ground and / or the grinding vessel. Some materials are so temperature-sensitive that they cannot be ground to the desired quality in current laboratory grinding media mills. Other materials can only be ground after becoming brittle. The grinding vessels themselves may also be subject to thermal or pressure limitations, especially if they are joined. Furthermore, safety precautions for operation must be observed.

[0008] Patent DE 10 2006 047 481 describes a ball mill with a grinding vessel comprising two transducers, one of which is a temperature sensor and the other a pressure sensor, as well as a plate that can be positioned on the lid and supports at least one of the transducers. During operation of the ball mill, the transducer records at least one measured value of the condition inside the grinding vessel, in particular the pressure and / or temperature.

[0009] Patent application DE 10 2023 103 629 (not pre-published) describes a laboratory grinding media mill for comminuting material to be ground, wherein the grinding vessel is provided with, for example, a passive thermochromic display device at least in a visible area on the outside of the grinding vessel. General description of the invention

[0010] The object of the invention is to provide a laboratory grinding media 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.

[0011] A further aspect of the object of the invention is to provide a laboratory grinding media mill which simultaneously combines both automation and manual operation and which, particularly with increasing automation, can additionally provide the user with information about selected parameters of the material to be ground, the grinding atmosphere and / or the grinding vessels, in particular immediately after grinding, as quickly as possible and ergonomically.

[0012] A further aspect of the object of the invention is to provide a laboratory grinding media mill which is safe and ergonomic for the user to operate.

[0013] A further aspect of the object of the invention is to provide a laboratory grinding media mill which can control the processes taking place in the grinding vessel under different conditions at least partially automatically and / or can protect the grinding set and / or the material to be ground from undesired impairments.

[0014] A further aspect of the object of the invention is to provide a laboratory grinding media mill which provides the user with additional information about the grinding process.

[0015] A further aspect of the object of the invention is to provide a laboratory grinding media mill which can reconcile the grinding time, the energy input, user and material protection restrictions of the grinding vessels as well as requirements of different materials to be ground.

[0016] The object of the invention is achieved by the subject matter of the independent claims. Advantageous developments of the invention are defined in the dependent claims.

[0017] According to one aspect of the present invention, a laboratory-scale grinding media mill, i.e. a laboratory grinding media 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 media mill comprises a grinding vessel with a grinding bowl and a grinding bowl lid for hermetically sealing the grinding bowl. The grinding vessel can, for example, be largely cylindrical in design, so that the grinding bowl lid closes the grinding vessel axially at an opening on the front side relative to the grinding bowl axis. The grinding bowl lid itself can also be cup-shaped, in which case the grinding bowl and grinding bowl lid can interlock in a cup-like manner. The grinding vessel defines the interior of the grinding vessel, which can be filled with grinding material and grinding media, in particular grinding balls.By means of rotational and / or oscillating movements, i.e. a permanently changing acceleration of the grinding vessel, whereby the direction and / or amount of the acceleration can also permanently change, the material to be ground in the grinding vessel interior between the grinding bodies and the walls, e.g. a grinding bowl shell wall, a grinding bowl base and / or the grinding bowl lid, of the grinding vessel is ground by impact and friction effects and / or is subject to further physical-chemical reactions or processes.

[0018] During operation, the grinding vessel is firmly clamped into a grinding vessel holder of the laboratory grinding media mill in order to transfer the rotational and / or oscillating movements from the grinding vessel holder to the clamped and closed grinding vessel.

[0019] An electric motor drives the rotation and / or oscillation of the grinding vessel holder with the grinding vessel clamped therein. For example, in a planetary ball mill, the electric motor can drive the sun and planetary rotation at a specific speed ratio via a belt drive, as shown in the documents listed in the introduction, e.g., on planetary ball mills, which are hereby incorporated by reference.

[0020] The laboratory grinding media mill has, in particular, in its stationary mill housing, a mill control device which controls the grinding process, e.g., drive parameters such as speed, oscillation frequency, grinding time, etc. of the laboratory grinding media mill. The mill housing also houses the moving parts of the laboratory grinding media mill, such as the grinding vessel holding device and the grinding vessel clamped therein. Preferably, the mill housing has an openable and closable housing cover which protects the moving parts from access during operation and allows access to the grinding vessel by opening the housing cover when the laboratory grinding media mill is stationary. The laboratory grinding media mill has, in particular, a safety circuit which ensures that the grinding process can only be started when the housing cover is closed.

[0021] 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 the interior of the grinding vessel 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 for the user directly on the outer side of the grinding vessel.

[0022] With the electronic display device directly on the grinding vessel, a laboratory grinding media mill can provide a special and multiple benefit for the user.

[0023] Advantageously, the user can have the desired information about the status parameter directly in the grip and line of sight of the grinding vessel, regardless of whether the grinding vessel is still clamped in the grinding vessel holding device or whether the grinding vessel clamping device has already been opened.

[0024] This prevents, among other things, the user from touching the grinding vessel with bare fingers when operating the grinding vessel clamping device if the temperature exceeds a certain threshold, without the user having to look away, for example, at a user interface on the laboratory grinding media mill or elsewhere on the mill. The same applies when removing the grinding vessel from the grinding vessel holding device or from the laboratory grinding media mill. This provides the user with the relevant information and warning functions exactly where they would typically place their fingers and where a potential hazard could arise, and does not require them to look away.

[0025] Furthermore, during the grinding process, depending on the material being ground and the energy input, not only a high temperature but also a high gas pressure can build up in the grinding vessel. The grinding vessel is often opened outside the mill, e.g. away from the mill on a laboratory bench, namely after the user has already removed the grinding vessel, possibly wearing protective gloves. In such laboratory situations, the user can, for example, be protected from an explosive escape of the gas atmosphere from the interior of the grinding vessel when the grinding vessel is opened if the user is shown the gas pressure directly on the grinding vessel itself. The user therefore always has the relevant information and warning functions in the right place, regardless of how the grinding vessel is handled.It may also be relevant for the user to have the gas temperature inside the grinding vessel and / or the contact temperature of the grinding vessel outside the mill in their field of vision if the grinding vessel is being handled outside of or away from the laboratory grinding media mill, e.g. if it is to be opened. The user therefore has information about the measured condition parameter of the inside of the grinding vessel in their field of vision in the direction of their grasp at any time and regardless of how the grinding vessel is being handled, even if the grinding vessel has already been removed from the laboratory grinding media mill and, for example, has been placed on a laboratory bench or in a fume cupboard in order to open it and remove the material to be ground. If necessary, the user can also draw specific conclusions about the material to be ground, the gas atmosphere inside the grinding vessel and / or the behavior when the grinding vessel is opened from the presence of several pieces of information in combination, such as gas pressure, gas temperature and / or contact temperature.

[0026] If necessary, the user can distinguish or identify multiple grinding vessels from the same or different laboratory grinding media mills after grinding by reading the measured condition parameter on the grinding vessel. For example, with the same weight but different input parameters, different temperatures may develop, e.g., with different grinding material or with wet grinding versus dry grinding.

[0027] Preferably, the grinding vessel comprises a power supply for supplying the electronic display device of the grinding vessel with electrical energy, e.g. in the grinding bowl lid.

[0028] The at least one sensor is, in particular, a temperature sensor and / or a pressure sensor. This allows the current temperature and / or pressure in the grinding vessel to be displayed, which can provide safety-relevant information when removing the grinding vessel from the laboratory grinding media mill and when opening the grinding vessel.

[0029] The grinding vessel may preferably comprise a grinding bowl base, a circumferential grinding bowl shell wall in the form of an annular wall surrounding the grinding bowl axis or grinding vessel axis, and the grinding bowl lid, wherein the at least one sensor comprises at least one or more of the following sensors: a gas temperature sensor which measures a temperature value of the gas atmosphere in the grinding vessel interior, a contact temperature sensor which measures a temperature measurement value of a grinding vessel wall, in particular the grinding jar bottom, the grinding jar shell wall or the grinding jar lid, by thermal contact, a pressure sensor that measures the gas pressure of the gas atmosphere in the grinding vessel interior.

[0030] Preferably, the grinding bowl base, the grinding bowl shell wall, or the grinding bowl lid has a measuring cavity and a connecting channel that connects the grinding vessel interior to the measuring cavity for fluid exchange and pressure equalization, thus ensuring fluid communication between the grinding vessel interior and the measuring cavity. The gas temperature sensor and / or the pressure sensor can be arranged in the measuring cavity, and the measuring cavity is fluidly connected to the grinding vessel interior via the connecting channel, so that the gas atmosphere in the measuring cavity is essentially the same as in the grinding vessel interior, and the pressure sensor and the temperature sensor provide the corresponding measured values ​​of the gas atmosphere of the grinding vessel interior.

[0031] Preferably, the grinding vessel comprises a grinding vessel circuit board with grinding vessel-specific control electronics, which has sensor readout 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 from the grinding vessel's power supply in order to read the at least one sensor directly on the grinding vessel and control the electronic display device on the outside of the grinding vessel, so that the status parameters measured by the at least one sensor are electronically displayed directly on the outside of the grinding vessel. Although this may increase energy consumption at the grinding vessel, it can simplify communication between the grinding vessel and the stationary mill control device.

[0032] The electronic display device can preferably be arranged on an outer surface of the grinding bowl lid, in particular on the upper side when clamped in place. This can be advantageous because, after opening the housing lid, the user's line of sight can, for example, fall directly onto the clamped grinding vessels.

[0033] Preferably, the grinding vessel has a central grinding vessel axis that centrally intersects the grinding vessel base and the grinding vessel lid, wherein the grinding vessel lid has an outer face and a circumferential surface surrounding the central grinding vessel axis, and wherein the outer face has a central face region and a peripheral annular 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 media mills, the clamping device of the grinding vessel holding device does not obstruct the view of the electronic display device when the grinding vessel is clamped in place.

[0034] According to one embodiment, the electronic display device comprises an alphanumeric digital display with a letter and / or number display and, in particular, displays the gas temperature measurement, the contact temperature measurement, and / or the pressure measurement, each as a numerical value. This data can be helpful to the user for further grinding vessel handling, particularly when combining various displayed status parameters.

[0035] 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, which are controlled by the grinding vessel's own control electronics.

[0036] Preferably, the mill control device and / or the grinding vessel's own control electronics have a memory which is designed to store one or more threshold values ​​for the state parameter to be measured.

[0037] According to one embodiment, the electronic display device may have at least one light-emitting element, e.g. an LED, which visibly lights up when the measured value of the state parameter measured by the at least one sensor exceeds the at least one stored threshold value.

[0038] If necessary, the grinding vessel can also comprise an acoustic signal generator which emits an acoustic warning signal when the measured value of the status 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 is so high that special safety precautions may be required during handling, in particular before opening the grinding vessel.

[0039] According to one embodiment, the mill control device or the grinding vessel's own control electronics can have a memory which is designed to store a plurality of threshold values ​​of different levels for the status parameter, wherein the electronic display device has a plurality of light-emitting elements, e.g. LEDs, which each successively light up visibly when the threshold values ​​of different levels for the status parameter are exceeded and / or wherein the grinding vessel comprises an acoustic signal generator which successively emits different acoustic warning signals when the threshold values ​​of different levels for the status parameter are exceeded in order to signal to the user that threshold values ​​of different levels have been exceeded.

[0040] According to one aspect of the invention, the laboratory grinding media 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.

[0041] The laboratory grinding media mill can also have a fluid cooling system with a stationary cooling fluid source, e.g., a vessel containing liquid nitrogen, from which a cooling fluid, e.g., liquid nitrogen (LN2), can 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 loop is formed in which the mill control device actively regulates the pressure and / or temperature in the interior of the grinding vessel in response to the state parameter measured by the at least one sensor by selectively dosing the cooling fluid.

[0042] In particular, the mill control device can, in response to the state parameter measured by the at least one sensor, in particular in response to the temperature and / or pressure measured by the at least one sensor, in particular in response to the temperature measured of the gas atmosphere in the grinding vessel interior, measured by the gas temperature sensor, control the rotation 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. The use of the gas temperature measured value has the advantage of demonstrating a rapid response, in particular a faster response than the measurement of a contact temperature.

[0043] The invention also relates to the grinding vessel, prepared for the laboratory grinding media mill, in particular as described above, comprising: a grinding bowl and a grinding bowl lid for closing the grinding bowl, wherein the grinding vessel defines a grinding vessel interior which can be filled with grinding material and grinding media, at least one sensor which measures a condition parameter of the grinding vessel and / or the grinding vessel interior and an electronic display device which is arranged on an outer side of the grinding vessel and which displays the condition parameter measured by the sensor visibly for the user directly on the outer side of the grinding vessel.

[0044] The invention further relates to the grinding bowl lid, prepared for placement on the grinding bowl to form a grinding vessel for the laboratory grinding media mill, in particular as described above, comprising: at least one sensor that measures a state parameter of the grinding vessel and / or the grinding vessel interior when the grinding bowl is closed with the grinding bowl lid, and an electronic display device which is arranged on an outer side of the grinding bowl lid and which displays the condition parameter measured by the sensor visibly for the user directly on the outer side of the grinding bowl lid.

[0045] The invention further relates to a method for controlling the laboratory grinding media mill as described above, wherein the same sensor, in particular pressure, gas temperature and / or contact temperature sensor, is used to control the laboratory grinding media 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.

[0046] According to a further aspect of the invention, a laboratory grinding media 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 that define and enclose a grinding vessel interior. The walls are formed, for example, by a grinding vessel base, a circumferential grinding vessel shell wall, and a grinding vessel lid, in particular a lid plate made of the material of the grinding vessel or the grinding vessel insert. The grinding vessel is hermetically sealed with the grinding vessel lid for the grinding process.The grinding bowl base, the grinding bowl 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 means of impact and friction effects by means of rotational and / or oscillating movements, in particular by means of permanently changing acceleration of the grinding vessel, with permanently changing direction and / or amount.

[0047] For this purpose, the grinding vessel is clamped into a grinding vessel holding device in order to transfer the rotational and / or oscillating movements from the grinding vessel holding device to the clamped and closed grinding vessel.

[0048] The grinding vessel holder, with the grinding vessel clamped within it, is driven by 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.

[0049] The laboratory grinding media mill further comprises a mill control unit in a stationary mill housing, which controls the grinding process, e.g., drive parameters such as speed, oscillation frequency, grinding time, etc. of the laboratory grinding media mill. The mill housing houses both the mill control unit and the moving parts of the laboratory grinding media mill. The mill housing is closed by a housing cover to allow the user access to the grinding vessel when the mill housing is open, e.g., to remove the grinding vessel, and to protect the moving parts from user access when the mill housing is closed.

[0050] The grinding vessel comprises a gas temperature sensor which measures a gas temperature measurement value of the gas atmosphere 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, i.e. in particular a contact temperature of the grinding vessel bottom, the grinding vessel shell wall or the cover plate through thermal contact with the wall.

[0051] The gas temperature measurement and the contact temperature measurement can provide different information about the grinding process. For example, during a phase transformation process, the gas temperature can rise or fall abruptly, while the contact temperature changes only slowly. This allows the grinding process to continue even if the gas temperature measurement briefly exceeds a critical threshold, as long as the contact temperature measurement does not, for example, measure a maximum permissible grinding bowl temperature that could damage a joined grinding bowl.

[0052] Also, possibly in combination with the pressure measurement, new insights into the chemical-physical processes taking place in the grinding vessel interior can be gained, among other things because the gas temperature in the grinding vessel interior and the contact temperature of the grinding vessel material can exhibit different temporal response behaviors during the grinding process.

[0053] Furthermore, the contact temperature can generally be used as an input variable for the start of the grinding process. For example, the user often has several grinding jars in use. Due to previous processes, there may already be a temperature difference between the grinding vessels before grinding. For example, grinding vessels may come from a dishwasher, an autoclave, or a previous grinding process and have been cleaned by hand, or grinding vessels may have previously been stored in a cabinet at room temperature. The resulting measured contact temperatures of the grinding vessels at the start of the grinding process can therefore already vary considerably. The grinding vessel temperatures at the start of grinding can influence the grinding process and, particularly when compared with the gas temperature, can provide the user with beneficial insights into the grinding process.

[0054] Preferably, the walls of the grinding vessel comprise a grinding bowl base, a grinding bowl shell wall running around the grinding vessel axis and a grinding bowl lid, and the gas temperature sensor and / or the contact temperature sensor can be arranged and fastened in or on the grinding bowl lid.

[0055] Preferably, the grinding vessel, in particular the grinding bowl 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 measure the gas temperature of the gas atmosphere in the grinding vessel interior.

[0056] The contact temperature sensor is in direct thermal contact with one of the walls of the grinding vessel and measures the contact temperature value of the respective wall by means of the thermal contact.

[0057] The mill control device in the mill housing is preferably arranged to receive the gas temperature measurement and the contact temperature measurement from the grinding vessel and to control the grinding process in response to the temperature measurements of both sensors, ie in response to the gas temperature measurement measured by the gas temperature sensor and to the contact temperature measurement measured by the contact temperature measurement.

[0058] The mill control device can in particular be designed 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.

[0059] Preferably, the grinding vessel also comprises a pressure sensor which measures the gas pressure of the gas atmosphere in the grinding vessel and sends it to the mill control device.

[0060] According to one embodiment, the stationary mill control device may be configured to compare the gas temperature measurement and the contact temperature measurement and to control the milling process in response to the temperature comparison and in response to the gas pressure measurement.

[0061] The walls of the grinding vessel can, in particular, comprise a grinding bowl base, a circumferential grinding bowl shell wall, and a grinding bowl lid, preferably with a lid plate made of a material that withstands the impact and friction effects of the grinding media and the material to be ground, in particular made of the material of the grinding bowl or the grinding bowl insert. The grinding bowl base, the grinding bowl shell wall, or the grinding bowl lid further comprise a measuring cavity and a connecting channel through the lid plate to connect the grinding vessel interior to the measuring cavity for fluid communication. The gas temperature sensor, the contact temperature sensor, and / or the pressure sensor are arranged in the measuring cavity.

[0062] Preferably, the grinding vessel, e.g. in the grinding vessel lid, has a power supply and a grinding vessel circuit board with grinding vessel-specific control electronics and sensor readout electronics, to which the gas temperature sensor, the contact temperature sensor and / or the pressure sensor and the power supply are connected, if necessary via electrical connectors.

[0063] Furthermore, the grinding vessel can comprise an electronic display device, which is supplied with electrical energy from the power supply. The electronic display device is arranged or attached, in particular, to an outer side of the grinding vessel and displays the gas temperature measurement and / or the contact temperature measurement directly on the outer side of the grinding vessel, visible to the user.

[0064] The walls of the grinding vessel comprise in particular a grinding bowl base, a circumferential grinding bowl shell wall and a grinding bowl lid, and the electronic display device is preferably arranged on an axially frontal or upper outer surface of the grinding bowl lid.

[0065] Furthermore, the grinding vessel can have a central grinding vessel axis which intersects the grinding vessel bottom and the grinding vessel lid centrally, wherein the grinding vessel lid has an end-side outer surface and a circumferential or tangential shell surface, and wherein the electronic display device is arranged on the end-side outer surface of the grinding vessel lid.

[0066] The mill control device or the grinding vessel board may comprise a memory 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.

[0067] Furthermore, the stationary mill control device can be configured to stop the milling process and / or to reduce the rotation or vibration frequency of the mill vessel receiving device when the gas temperature measurement value exceeds the first threshold value and / or when the contact temperature measurement value exceeds the second threshold value, wherein the first and the second temperature threshold values ​​are of different levels.

[0068] Preferably, the laboratory grinding media mill 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 grinding vessel's own control device to the stationary mill control device or an external computer.

[0069] According to one aspect of the invention, the laboratory grinding media mill can have a fluid cooling system with a stationary cooling fluid source, e.g., a vessel containing liquid nitrogen, from which the cooling fluid can be supplied to the moving grinding vessel. The cooling fluid can, for example, be introduced onto 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 then controlled by the mill control device, in particular to form a control loop in which the mill control device actively regulates the pressure and / or the temperature in the grinding vessel in response to the gas temperature measured by the gas temperature sensor and / or the contact temperature measured by the contact temperature sensor, in particular in response to a comparison of the gas temperature measured and the contact temperature measured, by targeted dosing of the cooling fluid.

[0070] In particular, the mill control device can, 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, control the rotation 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.

[0071] The invention also relates to the grinding vessel, prepared for the laboratory grinding media 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 bowl and a grinding bowl lid for closing the grinding bowl, wherein the grinding vessel defines a grinding vessel interior which can be filled with grinding material and grinding media, a gas temperature sensor which measures a gas temperature value of the gas atmosphere in the grinding vessel and a contact temperature sensor that measures a contact temperature reading of one of the walls of the grinding vessel.

[0072] The invention also relates to the grinding bowl lid, prepared for placement on a grinding bowl to form the grinding vessel for the laboratory grinding media mill, in particular planetary ball mill, centrifugal ball mill or vibrating mill, in particular as described above, wherein the grinding bowl lid comprises a control device in an electronics interior in the grinding bowl lid and a gas temperature sensor and (i) a contact temperature sensor that measures a contact temperature reading of the grinding bowl lid or (ii) an electrical connector for electrically contacting a contact temperature sensor by means of a complementary electrical connector of the grinding bowl, in order to measure a contact temperature reading of one of the walls of the grinding bowl with the contact temperature sensor and to read 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 bowl lid is placed on the grinding bowl.

[0073] The invention further relates to a method for controlling a laboratory grinding media 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 bowl with grinding material and, if necessary, one or more grinding media, Closing the grinding bowl with an associated grinding bowl lid to form a closed filled grinding vessel, wherein the grinding bowl or the grinding bowl lid has a gas temperature sensor and wherein the grinding bowl or the grinding bowl lid has a contact temperature sensor, Inserting (before or after closing the grinding vessel) and clamping the grinding vessel in a grinding vessel holder device of the laboratory grinding media mill, Closing the mill housing, Pre-selection of grinding parameters, in particular grinding time and / or rotation or oscillation frequency of the grinding vessel holding device by means of a user interface of the laboratory grinding media mill, Starting the grinding process, 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, and wherein 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.

[0074] Preferably, the mill control device aborts 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 time preselected by the user, reduces the rotation 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.

[0075] The invention is explained in more detail below using exemplary embodiments and with reference to the figures, wherein identical and similar elements are partially provided with the same reference numerals and the features of the various exemplary embodiments can be combined with one another. The following exemplary embodiments are designed identically in many aspects, so that features described with reference to one exemplary embodiment should also be considered as disclosed for the other exemplary embodiments, unless explicitly described otherwise or obviously different. Short description of the characters

[0076] They show: Fig. 1 an exploded view of an embodiment of the grinding vessel, Fig. 2 a cross-sectional view of the closed grinding vessel from Fig. 1, Fig. 3 a cross-sectional view of an embodiment of the grinding vessel in monolithic construction, Fig. 4 a cross-sectional view of an embodiment of a joined grinding vessel, Fig. 5 an exploded view of an embodiment of a lid measuring unit, Fig. 6 a cross-sectional view through the lid measuring unit assembled into a structural unit from Fig. 5, Fig. 7 a three-dimensional view of the assembled lid measuring unit from Fig. 5, Fig. 8 a three-dimensional view of another embodiment of the grinding vessel, Fig. 9 a cross-sectional view of another embodiment of a joined grinding bowl, Fig. 10 a three-dimensional view of the grinding bowl from Fig. 9, Fig. 11 a cross-sectional view of another embodiment of a monolithic grinding bowl, Fig. 12 a three-dimensional view of the grinding bowl from Fig. 11, Fig. 13 an exploded view of an embodiment of a grinding vessel with the grinding bowl from Fig. 11, Fig. 14 a three-dimensional view from below when placing the lid measuring unit on a grinding bowl, Fig. 15 a three-dimensional view from above when placing the lid measuring unit on a grinding bowl, Fig. 16 a three-dimensional representation of an embodiment of a vibrating disc mill, Fig. 17 an enlarged detail representation from Fig. 16, Fig. 18 a three-dimensional representation of an embodiment of a planetary ball mill, Fig. 19 a partially cutaway view of the planetary ball mill from Fig. 18, Fig. 20 a block diagram of an embodiment of the grinding vessel's own control device. Detailed description of the invention

[0077] Referring to the Fig. 1-4, the grinding vessel 8 comprises a grinding bowl 10 and a grinding bowl lid 12 for closing the grinding bowl 10, in particular hermetically. In the present example, the grinding bowl lid 12 comprises an upper lid measuring unit 14 and a lid plate 16, which closes an upper axial opening 20 of the grinding bowl 10 and axially delimits the grinding vessel interior 18 relative to the lower front grinding bowl base 54. The grinding bowl lid 12 and the lid plate 16 are sealed against each other with a grinding vessel seal 22, in the present example an elastomeric ring (flat) seal, when the grinding bowl lid 12 is clamped to the grinding bowl 10. In the present example, the grinding bowl cover 12 is screwed to the grinding bowl 10, e.g. with screws 24 which engage in threaded holes 26 which are arranged on the upper side 10a of the grinding bowl 10 around the grinding bowl opening 20.The grinding vessel 8 for the laboratory grinding media mill 1 preferably has a feed volume of 2 ml to 1000 ml, preferably of 20 ml to 500 ml.

[0078] When the grinding vessel 8 is open, the grinding vessel interior 18 is accessible to the user through the grinding bowl opening 20 on the top side 10a, in order to fill the grinding material and grinding media (both not shown) through the grinding bowl opening 20. The grinding vessel seal 22 is then placed on a grinding bowl sealing rim 26, in particular on the front side, which runs around the grinding bowl opening 20. The cover plate 16, which closes the grinding vessel interior 18 at the front or at the top, is then placed on the grinding vessel seal 22. The user can do this by individually grasping the cover plate 16, e.g. by its grip ring 28. The cover measuring unit 14 can then be placed as a pre-assembled unit on the top side 10a of the grinding bowl 10 orplaced onto the grinding bowl opening 20 (covered by the cover plate 16) and screwed to the grinding bowl 10 with the screws 24, whereby the grinding vessel seal 22 is clamped between the cover plate 16 and the annular grinding bowl sealing surface 26 in order to hermetically seal the grinding vessel. However, it is also possible for the grinding bowl cover 12 comprising the cover plate 16 and the cover measuring unit 14 to be connected to one another in advance, for example, by clamping, in order to place the entire grinding bowl cover 12 including the cover plate 16 as a whole onto the grinding bowl 10.The grinding bowl lid 12 can thus be constructed in several parts, with the lid plate, which defines the grinding vessel interior 18 and is preferably made of the same material as the inner walls of the grinding bowl 10, and the lid measuring unit, which houses the electronic components of the grinding bowl lid 12 and can, in particular, also contain plastic components. The lid measuring unit 14 is therefore a type of measuring and electronics attachment of the grinding bowl lid 12.

[0079] The lid measuring unit 14 is screwed together as a pre-assembled unit with additional screws 30. The lid measuring unit 14 is designed in several parts and can comprise a lid base 32, which forms a sensor / electronics unit, for example with the sensor and / or the grinding jar electronics, an intermediate body 34, which houses the battery, for example, and / or an upper, in particular axially visible cover 36. The lid measuring unit 14 forms an electronics interior 38, in the present example between the lid base 32 and the intermediate body 34, which houses a grinding vessel circuit board 40 with grinding vessel-specific control electronics 64. A battery holder 42 can be fastened in the lid measuring unit 14, for example axially above the lid base 32 in the intermediate body 34, into which battery holder 42 an electrical power supply 44, for example in the form of a battery 45 for the grinding vessel-specific control electronics 64, is inserted.The axially visible cover 36, which axially or upwardly closes off the grinding bowl lid 12, is seated on the intermediate body or battery body 34. An electronic display device 46 is fastened to an outer side 9 of the grinding vessel 8, in the present example on the front outer surface or upper side 12a of the grinding bowl lid 12, in particular the lid measuring unit 14. In the present example, the electronic display device 46 is designed as a foil display 48, which is attached to the outer side 9 of the grinding vessel 8, here on the front outer surface 12a of the grinding bowl lid 12 or the surface 36a of the cover 36, e.g., in a central axial recess 37 (. Fig. 5, Fig. 13). The lid measuring unit 14 can also include an acoustic signal generator 47, which is controlled by the grinding vessel's own control electronics 64.

[0080] The electronic display device 46 can have an on / off switch 48, e.g. 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 12a of the grinding bowl lid 12, which in the present example is designed as a colored LED 52 that lights up when a temperature threshold is exceeded and is directly in the field of vision for the user when looking directly at the grinding vessel. The electronic display device 46 or the electronic temperature display 50 is therefore arranged directly on the outer side 9 of the grinding vessel 8, in particular of the grinding bowl lid 12 or the lid measuring unit 14. The electronic display device 46 orThe electronic temperature display 50 is therefore arranged in a direct line of sight onto the grinding vessel 8, namely directly on its outer side 9 or upper side 8a, both when the grinding vessel 8 is inserted into the laboratory grinding media mill 1 and clamped there, and when the grinding vessel 8 is removed from the laboratory grinding media mill 1. This prevents, among other things, the user from touching the grinding vessel 8 after the grinding process without protective measures, without having to look at a display arranged elsewhere, in particular to avoid burns or other hazards.

[0081] In this example, the grinding vessel 8 is designed to be substantially rotationally symmetrical about a grinding vessel axis X. The grinding bowl 10 has an axially end-face grinding bowl base 54 through which the grinding vessel axis X extends substantially centrally. At a peripheral edge 54a of the grinding bowl base 54, the latter can be connected, in particular integrally, to the grinding vessel shell wall 56, which extends axially annularly around the grinding vessel axis from the grinding bowl base 54 to the grinding bowl opening 20. The annular grinding bowl sealing surface 26 can form an upper axial annular end face of the grinding bowl 10. The grinding bowl cover 12 can have an end-face upper outer surface 12a and a shell surface 12b extending around the grinding vessel axis X.

[0082] The grinding vessel board 40 can be clamped into the lid base 32 from above with an O-ring 58, e.g., the lid base 32 has an inner recess 33, which can form the electronics interior 38. A sensor device 60, in this example a combined pressure and temperature sensor 62, 80, can be attached to the underside 40a of the grinding vessel board 40. The sensor device 60 is read by the grinding vessel's own control electronics 64, e.g., with a microcontroller 242.

[0083] In the present example, the sensor device 60 comprises a piezoresistive pressure transmitter with an integrated microcontroller interface. For example, a sensor device 60 with a welded, oil-filled stainless steel housing 61 can be used, in which the sensor's own microcontroller interface is housed. Such pressure transmitters have, in particular, low power consumption, which is particularly advantageous in this case due to the limited space available when battery-operated. The sensor device 60 is delimited on the measuring side by a pressure diaphragm 68. The pressure diaphragm 68 is in gas contact with a measuring cavity 70 in which the gas pressure and gas temperature are measured. The sensor device 60 can be arranged in an annular sleeve 78 of the lid base 32. In the present example, the measuring cavity 70 is arranged in an interior space of the grinding bowl lid 12 and hermetically sealed against the outside 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 here (axially) delimited on the grinding bowl side by the upper side 16b of 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, e.g., 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 measuring cavity 70 is radially sealed by a measuring cavity sealing ring 76, which can rotate radially around the measuring cavity 70 and is designed as an O-ring in the present example.In the present example, the measuring cavity seal 76 seals radially against the annular sleeve 78 of the lid base 32, in which the sensor device 60 or the pressure sensor 62 can be arranged, and against the handle ring 28. In the present example, the measuring cavity 70 is located between the lid measuring unit 14 and the lid plate 16 and is delimited by the pressure membrane 68.

[0084] In the present example, the sensor device 60 comprises a gas temperature sensor that measures the gas temperature in the measuring cavity 70 and thus, via the fluid communication with the grinding vessel interior 18, also the gas temperature of the gas atmosphere located in the grinding vessel interior 18. In the present example, the first temperature sensor, which is designed as a gas temperature sensor 80, is integrated into the sensor device 60 with the pressure sensor 62. The gas temperature sensor 80 therefore does not measure the material temperature of solid parts of the grinding bowl lid 12 or the grinding bowl 10 by means of thermal contact, but rather measures the gas temperature of the gas located in the measuring 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 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 be measured. The measurement of the gas temperature is essentially not impaired even 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.

[0085] The pressure sensor 62 and the gas temperature sensor 80 are read by the grinding vessel's own control electronics 64, i.e., particularly within the grinding vessel as it accelerates during operation. The measured pressure and / or temperature values ​​can therefore be displayed both on the electronic display device 46 directly on the grinding vessel 8 ( Fig. 7) as well as with a transmitting device 65 of the grinding vessel's own control electronics 64 to a stationary receiving device 222 of the mill control device 224 ( Fig. 19). Thus, the pressure and temperature measured values ​​can be used in two ways, namely directly at the grinding vessel 8, whereby the user can measure the measured values ​​with the mill housing 204 open ( Fig. 16-18) the pressure and / or temperature information can be read directly on the grinding vessel 8, possibly even in alphanumeric and / or luminous form, and secondly as a control parameter for controlling the grinding process by the control device for controlling the laboratory grinding media mill 1.

[0086] Fig. 2 shows the grinding vessel 8 with an outer casing 82, for example made of stainless steel, and an inlay 84, for example made of agate or ceramic, e.g. zirconium oxide, defining the grinding vessel interior 18. The cover plate 16 is preferably made of the same material as the inlay 84, but in any case of a material that withstands the impact and friction of the material to be ground and, if applicable, the grinding media during operation, in order to form an inner wall 86 of the grinding vessel 8, if applicable made of a uniform material, defining and enclosing the grinding vessel interior 18. The grinding media (not shown) can be made of the same material as the inlay 84 or of a different material, which is selected based on the grinding task. The grinding vessel 8 and the grinding media together form the so-called grinding set.

[0087] Referring to Fig. 3 shows a monolithic grinding vessel 8. The monolithic grinding bowl 10 is made of stainless steel, for example. In this case, the cover plate 16 is also preferably made of stainless steel. Otherwise, the grinding vessel 8 corresponds to Fig. 3 the one from Fig. 2, so that reference can be made to it.

[0088] Referring to Fig. 4 is again a joined grinding vessel 8, similar to the one from Fig. 2, wherein the grinding vessel 8 is Fig. 4 also has a secondary or alternative measuring cavity seal 76'. The secondary or alternative measuring cavity seal 76' is designed, for example, as an elastomeric annular flat seal and seals the cover base 32 in a peripheral annular region against the cover plate 16.

[0089] Referring to Fig. 5-7, the electronic display device 46 can comprise an alphanumeric pressure display 88 and / or an alphanumeric temperature display 90, which the user can read directly on the outside of the grinding vessel 8, preferably the grinding bowl lid 12, when the mill housing 204 is open. The alphanumeric pressure or temperature displays 88, 90 have the advantage that the user is not only informed when a threshold value has been exceeded, but can also 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 display 88 displays the pressure measurement value measured by the pressure sensor 62. The alphanumeric temperature display 90 displays the gas temperature measurement value measured by the first temperature sensor, i.e., the gas temperature sensor 80.The electronic pressure and / or temperature displays 88, 90 can be controlled by the grinding vessel's own control electronics 64 and / or supplied with electrical energy by the grinding vessel's own electrical energy supply 44, in the present example in the form of the battery 45.

[0090] The grinding vessel circuit board 40 has an electrical (plug-in) connector 92 on its flat side (top side) 40b facing away from the grinding vessel interior. The plug-in connector 92 projects 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. A complementary electrical (plug-in) connector is arranged, in particular, on the underside 46b of the electronic display device 46. In the assembled state, the plug-in connector 92 is connected to the complementary plug-in connector 98 of the electronic display device 46 in order to control the electronic display device 46. The electrical connection through the two plug-in connectors 92, 98 also enables the switching on and off of the grinding vessel's own control electronics 64 by means of the switch 48.

[0091] Referring to Fig. 8, the electronic display device 46 may also comprise a plurality of simple LEDs 102, which may have different colors and indicate the exceeding of predefined temperature measurement values.

[0092] Referring to Fig. 9-10, the grinding vessel 8 can comprise a second temperature sensor, which is designed 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 bowl 10. The grinding bowl 10 has a recess 112 into which the contact temperature sensor 110 is inserted. In the present example, the grinding bowl 10 is joined, and the stainless steel holder 82 has a radial bore 114 into which the contact temperature sensor 110 is inserted radially from the outside and thermally contacts the inlay 84. In this way, the material temperature of the grinding bowl 10, here more precisely the grinding bowl inlay 84, can be measured, which has a high heat capacity. The temporal development of this material temperature during the grinding process can have a significantly different temporal characteristic than the gas temperature in the grinding vessel interior 18 or.of the measuring cavity 70, which is measured with the gas temperature sensor 80. From a comparison of the gas temperature measurement and the contact temperature measurement measured at the large heat capacity, useful additional information about the grinding process can be obtained and / or used to control the laboratory grinding media mill 1. The laboratory grinding media mill 1 can be controlled, in particular, in response to a comparison of the gas temperature measurement and the contact temperature measurement.

[0093] The contact temperature sensor 110 is connected to an electrical (plug-in) connector 120 via sensor connecting conductors 116, which run, for example, in a bore 118 inside the grinding vessel wall. In the present example, the plug-in connector 120 is arranged on the open axial end face of the grinding bowl 10, for example, on an annular edge 21 surrounding the opening 20, which simplifies the connection to a complementary (plug-in) connector. The contact temperature sensor 110 is preferably arranged on the grinding vessel or grinding bowl shell wall 56 in an axial edge region. In the present example, the contact temperature sensor 110 is arranged in an axial edge region 122 adjacent to the grinding bowl opening 20. Alternatively, the contact temperature sensor 110 can also be arranged in an axial edge region 124 of the grinding bowl shell wall 56 adjacent to the grinding bowl base 54.It has been shown that positioning the contact temperature sensor 110 away from the axial center 126 of the grinding bowl shell wall 56 can offer advantages with regard to the temperature distribution and the temporal temperature profile during the grinding process. However, it should not be ruled out that the contact temperature sensor 110 can be arranged in a central region 126 of the grinding bowl shell wall 56, on the grinding bowl base 54, or on the grinding bowl lid 12, in particular on the lid plate 16, and thermally contacted to measure the contact temperature of solid parts of the grinding vessel 8.

[0094] Referring to Fig. 11-12 illustrates a monolithic grinding bowl 10. Here, too, the contact temperature sensor 110 can be arranged in a radial bore 114 in the outer side 56b of the grinding bowl shell wall 56 and be in thermal contact therewith in order to directly measure the contact temperature of the grinding bowl 10.

[0095] Referring to Fig. 13-15, the plug connector 120 of the contact temperature sensor 110 is electrically connected to a complementary plug connector 128. In the present example, the electrical connection between the contact temperature sensor (plug) connector 120 and the complementary contact temperature sensor (plug) connector 128 is established automatically when the grinding bowl cover 12 is placed on the grinding bowl 10. The grinding bowl cover 12, or more precisely the cover measuring unit 14 and the grinding bowl 10, has an anti-twist device 130 that protects the plug contacts 132 of the plug connection 120, 128 from damage and ensures the correct orientation of the grinding bowl cover 12 relative to the grinding bowl 10 when establishing the electrical plug connection between the grinding bowl 10 and the grinding bowl cover 12.

[0096] Referring to Fig. 16-19, the laboratory grinding media mill 1, according to Fig. 16-17 for example as a vibrating disc mill 202 and according to Fig. 18-19, for example, designed 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 oscillating 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 enter 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 time. The display 210 can also display the measured pressure and / or temperature values, which are transmitted from the transmitting device 65 of the grinding vessel's own control electronics 64 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, the grinding time and / or the oscillation or rotation frequency, in response to the pressure and / or temperature measured values ​​transmitted by the grinding vessel's own control electronics 64. For example, the mill control device 224 can shorten the grinding time and / or reduce the oscillation or rotation frequency, e.g., if the pressure and / or temperature measured values ​​exceed predetermined threshold values. In particular, the mill control device 224 can control the grinding process in response to a comparison of the contact temperature measured value and the gas temperature measured value. 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, e.g., in a range in which the quality of the joint between the socket 82 and the inlet 84 is not yet impaired.Furthermore, the gas temperature in the grinding vessel interior 18 typically rises considerably faster at the beginning of the grinding process than the material temperature of the grinding vessel 8 due to its high 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 insight into the grinding process and / or to control the grinding process. For example, phase transitions or reactions in the material to be ground can be detected more effectively during the grinding process than if only one of the two temperatures is measured.

[0097] The mill housing 204 further comprises an openable and closable housing cover 212, which, when closed, securely encloses the moving parts of the laboratory grinding media mill 1, and, when opened, provides the user with 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 media mill 1 or insert it into it. The housing cover 212 thus securely closes the mill interior 218, in which the grinding vessel 8 is located during operation. It is apparent to a person skilled in the art that, depending on the mill subtype, the laboratory grinding media mills 1 can have multiple grinding vessel receiving devices 216 into which multiple grinding vessels 8 can be clamped. Multiple grinding vessels 8 can also be clamped into the same grinding vessel receiving device 216.

[0098] In the example of the vibrating disc mill 202 ( Fig. 16-17), the grinding bowl 10 is inserted into the laboratory grinding media mill 1 and, in the inserted state, filled with grinding material and grinding media. Subsequently, the grinding bowl lid 12 with the electronic display device 46 is placed on top and clamped with a grinding vessel clamping device 214. In a vibrating mill 202, the grinding vessel holding device 216 oscillates back and forth, for example, in a circular or linear motion, thus causing the grinding material to be crushed in the grinding vessel 8.

[0099] The planetary ball mill 302 ( Fig. 18-19), as with vibratory mills with smaller grinding vessels, the grinding vessel 8 can be filled and, if necessary, closed away from the laboratory grinding media mill 1 and inserted into the laboratory grinding media mill 1 already filled and, if necessary, closed. Referring to Fig. 18, the planetary ball mill 302 also has 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 to close the mill interior 218. In the illustrated planetary ball mill 302, the grinding vessel receiving device 216 rotates about the planetary axis, which coincides with the grinding vessel axis X, and the grinding vessel receiving device 216 rotates with the inserted grinding vessel 8 about a sun axis to generate a combined planetary motion when the planetary ball mill 302 is in operation.

[0100] Again referring to all types of the laboratory grinding media mill 1, when the housing cover 212 is opened, the user immediately sees the electronic display device 46 of the grinding vessel 8 and has access to the grinding vessel 8 in order to remove it from the laboratory grinding media mill 1 and / or to open and fill it.

[0101] The grinding process of the laboratory grinding media mill 1 can be controlled in response to the pressure measurement, gas temperature measurement, and / or contact temperature measurement 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 time and / or, in the case of the planetary ball mill 302, the rotation frequency of the grinding vessel receiving device 216 and / or the sun disk 220, or, in the case of a vibrating mill, the oscillation frequency, can be controlled in response to one or more of these measured values. In particular, the grinding parameters, such as the grinding time, 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 measurement and the contact temperature measurement.

[0102] Referring to Fig. 20, the grinding vessel's own control electronics 64, which is accelerated during operation with the grinding vessel, has a controller 242, which reads 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 into a common sensor device 60, which is arranged inside the grinding bowl lid 16 and forms an internal sensor device 60. In the examples shown, the contact temperature sensor 110 is arranged outside the measuring cavity 70 and forms an external sensor. The grinding vessel's own control electronics 64 transmits the measured values ​​measured by the sensors 62, 80, 110 via the (radio) transmitter device 65 to the stationary receiver device 222 of the mill control system 224. The threshold values ​​are stored in the configuration memory 244 and are read by the controller 242.The grinding vessel's own control electronics 64 further comprises a battery management module 246 and the controller is supplied with electrical energy by the battery 45.

[0103] When controlling the grinding process, the mill control device 224 can, in response to one or more of the measured values, possibly even override the setpoints specified by the user, for example by prematurely terminating the grinding process, shortening the duration of grinding cycles, or automatically reducing the rotation or oscillation frequency compared to the user specification. The mill control device 224 can thus automatically react to undesired or unexpected deviations of one or more 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 on the grinding vessel 8, from predefined parameters. Furthermore, the measured pressure value, the measured gas temperature value, and / or the measured contact temperature value can be visually displayed for the user directly on the grinding vessel 8 by means of the electronic display device 46 on the grinding vessel's own.This allows the user to obtain ergonomically precise information about the grinding process. Furthermore, the user can be prevented from touching the grinding vessel 8 with bare fingers if it exceeds a certain temperature threshold, without having to look at the user interface 206 of the laboratory grinding media mill 1 or at another location on the mill. This provides the user with the relevant information and warning functions precisely where a potential hazard might arise, which can provide a safety advantage.

[0104] Furthermore, the user can also be protected, for example, from an explosive escape of the gas atmosphere from the grinding vessel interior 18 when opening the grinding vessel 8 if the user has the gas pressure displayed directly on the grinding vessel 8 itself. This is particularly advantageous if the grinding vessel 8 is opened away from the laboratory grinding media mill 1. Nevertheless, the user has the relevant information and warning functions in the right place. If necessary, the user can also see the gas temperature and / or the contact temperature when the grinding vessel is removed from the laboratory grinding media mill 1 and handled, e.g., opened, away from it.

[0105] The laboratory grinding media mill 1, regardless of its type, can further comprise an integrated fluid cooling system 230 with a stationary cooling fluid source, which supplies cooling fluid to the grinding vessel 8 from a fluid nozzle 232 during the grinding process. Fig.16, this is schematically illustrated using the example of a vibratory mill 202, wherein the cooling fluid, e.g., liquid nitrogen, can be dripped from the fluid nozzle 32 onto the grinding vessel 8 during the grinding process. Alternatively, fluid channels can also be provided which supply the cooling fluid to the grinding vessel receiving device 216 and / or the grinding vessel 8. The fluid cooling can be implemented in a planetary ball mill, e.g., 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.

[0106] The quantity or dosage of the cooling fluid can also be controlled in response to one or more of the measured values, including the pressure measured value, the gas temperature measured value and / or the contact temperature measured value, which are measured with one or more of the sensors 62, 80, 110, in particular in response to a comparison of the gas temperature measured value and the contact temperature measured value.

[0107] It will be apparent to those skilled in the art that the embodiments described above are to be understood as examples and that the invention is not limited to them, but can be varied in many ways without departing from the scope of the claims.

[0108] It is furthermore apparent that the features, regardless of whether they are disclosed in the description, the claims, the figures or otherwise, also individually define essential components of the invention, even if they are described together with other features. In particular, it is apparent to a 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 independently of one another or combined with one another and are to be mutually deemed to be disclosed. Orientation indications such as top, bottom, left, right, front, rear, etc. relate to the figures used and are not to be understood as being absolutely limiting. For example, grinding vessels which are shown upright in some laboratory grinding media mills can also be inserted into the laboratory grinding media mill in a lying position, i.e. with the grinding vessel axis horizontal.The phrase "comprises" is an open list 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, can be provided for each receiving device, e.g., stacked. QUOTES CONTAINED IN THE DESCRIPTION

[0000] This list of documents submitted by the applicant was generated automatically and is included solely for the convenience of the reader. This list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions. Cited patent literature

[0000] DE 197 12 905 A1

[0002] DE 10 2006 006 529 A1

[0002] DE 10 2006 018 325 A1

[0002] DE 10 2006 047 481 A1

[0002] DE 10 2006 047 480 A1

[0002] DE 10 2006 047 479 A1

[0002] DE 10 2006 047 498 A1

[0002] DE 10 2010 044 254 A1

[0002] DE 10 2012 009 983 A1

[0002] DE 10 2012 009 985 A1

[0002] DE 10 2012 009 982 A1

[0002] DE 10 2012 009 984 A1

[0002] DE 10 2012 009 987 A1

[0002] DE 10 2006 047 481

[0008] DE 10 2023 103 629

[0009] DE 20 2005 015 897 A1

[0105] DE 10 2020 127 234 A1

[0105] DE 10 2020 127 239 A1

[0105] DE 10 2020 127 240 A1

[0105]

Claims

[1] Laboratory grinding media mill (1), in particular planetary ball mill, centrifugal ball mill or vibrating mill, comprising: a grinding vessel (8) with a grinding bowl (10) and a grinding bowl lid (12) for closing the grinding bowl (10), wherein the grinding vessel (8) defines 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 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 in the laboratory grinding media mill (1), wherein the grinding vessel (8) comprises: at least one sensor (62, 80, 110) which measures a state parameter of the grinding vessel (8) and / or the grinding vessel interior (18), an electronic display device (46) which is arranged on an outer side (9) of the grinding vessel (8) and which displays the state parameter measured by the sensor (62, 80, 110) visibly for the user directly on the outer side of the grinding vessel. [2] Laboratory grinding media mill (1) according to claim 1, wherein the grinding vessel comprises a power supply (44) for supplying the electronic display device (46) of the grinding vessel (8) with electrical energy. [3] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the at least one sensor (62, 80, 110) comprises a temperature sensor (80, 110) and / or a pressure sensor (62). [4] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the grinding vessel (8) has a grinding bowl base (54), a circumferential grinding bowl shell wall (56) and a grinding bowl lid (12), and the at least one sensor (62, 80, 110) comprises at least one or more of the following sensors: a gas temperature sensor (80) which measures a gas temperature measurement value of the gas atmosphere in the grinding vessel (8), a contact temperature sensor (110) which measures a contact temperature measurement value of the grinding bowl bottom (54), the grinding bowl shell wall (56) or the grinding bowl lid (12), a pressure sensor (62) which measures the gas pressure of the gas atmosphere in the grinding vessel (8). [5] Laboratory grinding media mill (1) according to claim 4, wherein the grinding bowl base (64), the grinding bowl shell wall (56) or the grinding bowl lid (12) has a measuring cavity (70) and a connecting channel (72) which connects the measuring cavity (70) to the grinding vessel interior (18), wherein the gas temperature sensor (80) and / or the pressure sensor (62) is arranged in the measuring cavity (70), and the measuring cavity (70) is in fluid communication with the grinding vessel interior (18) via the connecting channel (72) in order to be able to measure the gas temperature and / or the gas pressure of the gas atmosphere in the grinding vessel interior (18) via the measuring cavity (70). [6] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the grinding vessel (8) has a grinding vessel board (40) with grinding vessel-specific control electronics (64), to which the at least one sensor (62, 80, 110) and the electronic display device (46) are connected in order to read the at least one sensor (62, 80, 110) and to control the electronic display device (46) on the outside (9) of the grinding vessel (8) in order to display the state parameters measured by the at least one sensor (62, 80, 110) directly on the outside (9) of the grinding vessel (8). [7] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the electronic display device (46) is arranged on an outer surface of the grinding bowl lid (12). [8] Laboratory grinding media mill (1) according to claim 7, wherein the grinding vessel (8) has a central grinding vessel axis (X) which centrally intersects the grinding vessel base (54) and the grinding vessel lid (12), wherein the grinding vessel lid (12) has an end-side outer surface (12a) and a circumferential surface (12b) surrounding the central axis (X), wherein the end-side outer surface (12a) has an end-side central region and an end-side peripheral ring region around the central grinding vessel axis (X), wherein the electronic display device is arranged at a distance from the central grinding vessel axis (X). [9] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the electronic display device (46) comprises an alphanumeric digital display with a letter and / or number display. [10] Laboratory grinding media mill (1) according to claim 9, wherein the alphanumeric digital display comprises an LCD display, a TFT display, a QLED display, an OLED display, an AMOLED display or an electronic paper display, which are controlled by the grinding vessel's own control electronics (64). [11] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the mill control device (224) or the grinding vessel's own control electronics (64) have a memory (244) which is adapted to store at least one threshold value for the state parameter. [12] Laboratory grinding media mill (1) according to claim 11, wherein the electronic display device (46) has at least one luminous element (52, 102) which visibly lights up when the measured value of the state parameter measured by the at least one sensor (62, 80, 110) exceeds the at least one stored threshold value. [13] Laboratory grinding media mill (1) according to claim 11 or 12, wherein the grinding vessel (8) comprises an acoustic signal generator (47) which emits an acoustic warning signal when the measured value of the state parameter measured by the at least one sensor (62, 80, 110) exceeds the at least one stored threshold value. [14] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the mill control device (224) or the grinding vessel's own control electronics (64) have a memory (244) which is designed to store a plurality of threshold values ​​of different levels for the status parameter, wherein the electronic display device (46) has a plurality of light-emitting elements (102), which each successively light up visibly when the threshold values ​​of different levels for the status parameter are exceeded and / or wherein the grinding vessel (8) comprises an acoustic signal generator (47) which successively emits different acoustic warning signals when the threshold values ​​of different levels for the status parameter are exceeded. [15] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the laboratory grinding media mill (1) has a receiving device (222) and the grinding vessel (8) has a transmitting device (65) in order to transmit the state parameters measured by the at least one sensor (62, 80, 110) to the mill control device (224) or an external computer. [16] Laboratory grinding media mill (1), in particular planetary ball mill, centrifugal ball mill or vibrating mill, in particular according to one of the preceding claims, comprising: a grinding vessel (8) with a grinding bowl (10) and a grinding bowl lid (12) for closing the grinding bowl (10), wherein the grinding vessel (8) defines 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 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 milling process, wherein the grinding vessel (8) comprises at least one sensor (62, 80, 110) which measures a state parameter of the grinding vessel (8) and / or the grinding vessel interior (18), wherein the laboratory grinding media mill (1) has a receiving device (222) and the grinding vessel (8) has a transmitting device (65) in order to transmit the state parameters measured by the at least one sensor (62, 80, 110) to the mill control device (224), and wherein the mill control device (224) controls the laboratory grinding media mill (1) in response to the state parameters measured and transmitted by the at least one sensor (62, 80, 110). [17] Laboratory grinding media mill (1) according to one of the preceding claims, wherein the laboratory grinding media 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 interior (18) in response to the state parameter measured by the at least one sensor (62, 80, 110) by targeted dosing of the cooling fluid. [18] Laboratory grinding media mill (1) 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 quantity of the 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 (62, 80, 110), in particular in response to the gas temperature measurement value of the gas atmosphere in the grinding vessel (8) measured by the gas temperature sensor (80). [19] Grinding vessel (8) prepared for a laboratory grinding media 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 grinding bowl (10) and a grinding bowl lid (12) for closing the grinding bowl (10), wherein the grinding vessel (8) defines a grinding vessel interior (18) which can be filled with grinding material and grinding media, at least one sensor (62, 80, 110) which measures a state parameter of the grinding vessel (8) and / or the grinding vessel interior (18), an electronic display device (46) which is arranged on an outer side (9) of the grinding vessel (8) and which displays the state parameter measured by the at least one sensor (62, 80, 110) visibly for the user directly on the outer side (9) of the grinding vessel (8). [20] Grinding bowl lid (12) adapted to be placed on a grinding bowl (10) to form a grinding vessel (8) for a laboratory grinding media 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: at least one sensor (62, 80, 110) which measures a state parameter of the grinding vessel (8) and / or the grinding vessel interior (18), an electronic display device (46) which is arranged on an outer side (12a) of the grinding bowl cover (12) and which displays the state parameter measured by the at least one sensor (62, 80, 110) visibly for the user directly on the outer side (12a) of the grinding bowl cover (12). [21] Laboratory grinding media mill (1) according to one of claims 1-18 with a control which uses the same sensor (62, 80, 110) to control the laboratory grinding media mill (1) during operation with the measured state parameters and to visually display the measured state parameters to the user on the electronic display device (46) of the grinding vessel (8).

Images