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Author: Dr. Lena Weigold, Retsch GmbH.

A seemingly trivial but potentially challenging point in the homogenization of the sample is to keep the sample in its original state. For example, sample preparation in a ball mill is based on the physical mechanism of impact and friction. These two mechanisms lead to heat generation, which poses serious problems for temperature-sensitive materials. MM 500 control is the first laboratory ball mill specially designed to process temperature-sensitive materials.

The MM 500 controller monitors and controls the temperature of the grinding process. With a maximum frequency of up to 30 Hz, it is a powerful mill suitable for dry, wet and cryogenic grinding processes. In addition, the MM 500 controller uses an innovative sample cooling concept. The accessible temperature range covers the area from -100 to 100°C, providing a new method for sample cooling and cryogenic grinding, see Figure 1. The sample can even be heated.

In the MM 500 controller, the material is processed in Retsch screw-lock tanks, which are simply mounted on top of the hot plate for tempering (Figure 2). Since the grinding pot is in metal contact with the hot plate, the heat can be effectively transferred from or to the pot. The temperature of the hot plate is adjusted by the hot fluid in turn.

The technological innovation and advanced design of the MM 500 controller provide brand new functions, see also Figure 3. 1. Different configurations: The innovative internal piping system allows the use of liquid nitrogen or other hot fluids for sample tempering. Therefore, standard cryostats or liquid nitrogen tanks can be used for cooling. The low temperature can be reached for the first time without using liquid nitrogen. 2. Temperature monitoring: The actual temperature of the hot plate is continuously displayed during the grinding process, providing valuable information about the heat development in the tank. 3. Screw-lock tank: The screw-lock tank can use two tanks at the same time, and each tank has a maximum capacity of 125 ml, which can easily handle samples and achieve high throughput. Zirconium oxide and tungsten carbide grinding equipment can also be used for cryogenic grinding. 4. Hot plate: Allow indirect samples to be cooled and heated in the range of -100 to +100°C. 5. CryoPad technology: If liquid nitrogen is used for tempering, the optional cryoPad equipment extension must be used to extend the mill. For the first time, cryoPad technology allows the selection and maintenance of a specific cooling temperature for tempering. The accessible area for cooling with liquid nitrogen covers a range from -100 to 0°C in steps of 10. cryoPad's patented PID (Proportional Integral Derivative) system controls the flow of liquid nitrogen through the piping system and effectively regulates the temperature of the hot plate. 

Materials affected by thermal development exist in almost every application field. Agriculture, biology, chemistry, plastics, engineering, recycling, pharmacy, food industry, and even geology all require sample cooling, as shown in Table 1.

The MM 500 controller has the unique advantage of handling temperature-sensitive processes. There is no need for cumbersome sample pre-cooling or time-consuming grinding interruption to use this equipment. Regardless of the specific industry, four different goals have been identified that require sample cooling/heating: 1. Preservation of materials for analysis. If heated to high temperatures, the material may change its physical or chemical structure. This means that the target analyte is different from before the sample preparation. Looking at volatile substances or substances that evaporate at elevated temperatures, the amount of analyte will also change significantly due to heat generation.

2. The brittle toughness and viscous materials must be homogenized in a ball mill. Not all samples require a temperature of -196°C, such as the temperature reached in a typical cryogenic mill using liquid nitrogen. The MM 500 controller provides a convenient and safe cooling option with a high throughput that can be as low as -100°C.

3. Wet milling nano-grinding below room temperature is usually performed at high frequency/revolutions per minute in the wet milling process. The high energy input required usually results in temperatures above 80°C. If the jar is cooled with thermal fluid, there is no need to interrupt the cooling during this process and after sample preparation, see the example in Figure 5. Monitor the temperature of the heating plate throughout the process. Compared with other equipment, it is much easier to perform sub-sampling in a process to check the fineness. 4. The process of mechanochemical mechanochemistry and mechanical alloying requires energy to initiate or enhance the chemical reaction of materials or the formation of material mixtures. Active heating of the tank can significantly improve the result of the chemical reaction. On the other hand, the temperature adjustment of the MM 500 controller can also be used to maintain a selected temperature level throughout the process, thereby controlling the formation of chemical derivatives.

The Mixer Mill MM 500 controller is a truly world first: the first high-energy laboratory ball mill that can monitor and control the temperature during the grinding process. The mill provides new perspectives and possibilities for the homogenization of temperature-sensitive sample materials, cryogenic grinding or wet grinding processes, and mechanochemistry.

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