The polyBLOCK unit from HELgroup (www.helgroup.com) is a modular reaction platform allowing independent temperature control of four 200ml reaction vessels. Heating is achieved through use of a closed circuit heating coil and cooling is provided by a Huber unichiller. The use of a turbidity probe in each reactor allows for in-situ monitoring of dissolution/crystallisation events occurring in solution on application of heating or cooling. Alunimum adaptor blocks make possible the use of different volume reactors in the polyBLOCK; 20 4ml reaction vials or 3 10ml reactors can be accommodated in each vessel port. The turbidity probe cannot be used with the 4ml reactor.
LabmaxTM Reaction Vessel
The LabmaxTM is a 1L jacketed glass reaction vessel with automated heating, cooling and dosing controls. The vessel has an overhead impeller for agitation and a temperature sensor for temperature control. An offline pumping system offers the possibility of controlled reagent dosing in the course of a reaction. The entire unit is programmable from a desktop PC with iControlTM software. Used in conjunction with the FBRMTM, PVMTM and iC-10TM reaction probes, the system has the potential to monitor all aspects of a chemical reaction. Focused beam reflectance measurement (FBRMTM) in-situ reaction probe-The FBRM probe allows for in-situ particle size monitoring by tracking a cross section of particle size known as chord length. iC-10TM in-situ reaction probe- This probe provides in-situ infra red analysis of solutions, allowing monitoring of dissolved species. All the in-situ probes may be used in conjunction with the Labmax reaction vessel or independently in an off-line beaker or reaction vessel. All are controlled through PC with individual software programs.
Particle Visual Measurement(PVMTM)- The PVM is essentially a camera microscope which sits in solution and records particles as they evolve and grow.
X-ray Diffraction (XRD)
X-ray Diffraction (XRD) is used to investigate the structural characteristics of materials. XRD is a quantitative and qualitative technique which is used for 'fingerprint' characterisation of crystalline materials and their crystal structures. The diffraction pattern contains a range of peaks of different relative intensities at the specific angles of diffraction which is unique to a specific crystal structure. crystal phases can be identified from these diffraction patterns.
The basic operating principle of a FIB system is simliar to that of scanning electron microscopy, the major difference being the use of a gallium ion beam instead of an electron beam. The beam is raster-scanned over the sample, which is mounted in a vacuum chamber at pressures of approximately 5 x 10-6 mbar. When the beam strikes the sample, secondary electrons and secondary ions are emitted from the surface of the sample. The electron or ion intensity is monitored and used to generate an image of the surface. secondary electrons are generated in much larger quantities than ions and provide images of better quality and resolution; consequently, the secondary electron mode is used for most imaging applications. Ions beams can be use to remove material from the surface of the smaple. This is called Milling and is a major advatage of FIB as much of the constructional analysis and failure analysis of semiconductor is performed on cross-sections. FIB can aslo be used to deposit metals such as platinum and insulators such as silicon oxide.
Atomic Force Microscope (AFM)
The atomic force microscope (AFM) or scanning force microscope (SFM) is a very high-resolution type of scanning probe microscopy, with demonstrated resolution of fractions of a nanometer, more than 1000 times better than the optical diffraction limit. The AFM is one of the foremost tools for imaging, measuring and manipulating matter at the nanoscale. The information is gathered by "feeling" the surface with a mechanical probe. Piezoelectric elements that facilitate tiny but accurate and precise movements on (electronic) command enable the very precise scanning.
Raman Spectroscopy is sensitive to molecular and crystal structures and its applications include chemical fingerprinting, crystallite examination in ceramics and the examination of structure and strain rates in polycrystalline ceramics, glasses, fibers, gels and thin and thick films. the Dilor XY Labram spectrometer is equipped with an Olympics BX40 confocal microscope. An ArHe 10 mW green laser and a 20 mWred laser generate spectra that are collected with a peltiuer cooled CCD detector. For investigations between ambient temperatures and 1500 °C a LINKAM TS1500 temperature stage is used.