ProboStat™ Sample holder cell system for electrical and other characterization at high temperatures and under controlled atmospheres NorECs Norwegian Electro Ceramics AS
Outline 1. ProboStat™ 2. Base unit and accessories 3. Measurement setups 4. Other ProboStat™ related products NORECS AS
ProboStat™ ProboStat™ - a versatile sample holder for measurements of electrical properties, transport parameters, and kinetics of materials, solid/gas interfaces and electrodes at high temperatures under controlled atmospheres. Main features: Overall design: Single end fixture of all parts with closed end enclosing tube 40 mm outer diameter, 30-60 cm long Sample: 10-24 mm diameter disk 25-50 mm long bar Electrodes: 2, 3, or 4 Temperature: Typical long term: <1400 ° C shorter term: <1600 ° C Atmosphere: Oxidizing, inert, reducing, corrosive; Wet or dry Low vacuum 10 -2 mbar to atmospheric pressure (15 bar with enclosing steel tube) Single or dual chamber modes NORECS AS
ProboStat™ The ProboStat™ excels in easy exchange of samples and electrodes, and in versatility for many different methods NORECS AS
ProboStat™ Materials properties measured and applicable methods: Conductivity vs. T, p O 2 , p H 2 O, ect. I-V characteristics DC, AC, impedance spectroscopy Fuel cell component and single cell testing Dielectric properties, loss, ect. Electrode kinetics Disk, van der Pauw, and bar geometries Electrochemical pumping, gas 2, 3, and 4 electrodes permeation and electrocatalysis with gas analysis (e.g. GC or MC) on Ionic transport number outlets Proton transport number Sensor testing H/D isotope effect Poling of ferroelectrics possible with Seebeck coefficient the high-voltage (10 kV) version Annealing or sintering under controlled atmospheres NORECS AS
ProboStat™ base unit The base unit is the central unit in the ProboStat™ system The ProboStat™ base unit features: Ni-plated brass construction for good heat conduction (stainless steel option) O-ring sealed fixation of sample support tube and outer enclosing tube Spring load fixation collar 16 electrical feedthroughs (6 for electrodes, 4 for shields and 6 for thermocouples) 6 BNC electrode contact sockets 3 thermocouple contact sockets 3 toggle switches for grounding and shielding options 4 gas inlets/outlets with Swagelock quick- ProboStat™ base unit connects for two gas chambers cooling/heating water hose fittings NORECS AS
ProboStat™ base unit Gas inlet for inner chamber Gas outlet for inner chamber Socket for sample support tube Outer and inner electrical Gas inlet for outer chamber feedthroughs Gas outlet for outer chamber Water cooling / heating Thermocouple contact sockets BNC electrode contact sockets Gas inlets/outlets NORECS AS
ProboStat™ accessories The ProboStat™ system has a wide range of accessories designed for different types of electrochemical measurements NORECS AS
ProboStat™ accessories Outer enclosing tubes 40 mm outer diameter closed tubes of alumina or silica. Presently come in the standard designs for 10 – 24 mm Sample support tube diameter disks and for bar samples. assemblies Spring load assemblies Keeps sample and electrodes in contact and position. Come in variety of types. The standard material is high Electrode contact leads purity Pt. Other metals may be applied. Up to 3 thermocouples can be used. Thermocouples The type (commonly S or K) can be chosen by the user. Send gas directly to the sample area. Supply gases to Gas supply tubes the inner and outer chambers of the cell. NORECS AS
ProboStat™ accessories (optional) Temperature gradient across Crucible and sample plate holder Internal heater a bar sample as a function of power supplied to the internal A special support tube Can be used for heater. with a stop plate to hold creating 20 crucibles for annealing temperature 10 powders or samples, gradient in 318 oC o 0 T, and sintering under Seebeck -10 controlled atmospheres coefficient -20 or vacuum. measurements. 0 4 8 P, W Liquid cell assembly Top flange and open end outer tube The ProboStat™ system can Open end outer tube with be equipped with a liquid cell flange for evacuation and assembly to measure the optical access to disk dielectric constant of liquids at sample top surface/ RT – 200 ̊C. electrode. ... and more... NORECS AS
Standard ProboStat™ packages Options suitable for laboratories which value the cost- Extensively furnished version effectiveness of direct acquirement of new techniques without trial and error and development time. Normal plus version These examples may also be suitable systems for Normal version projects where a large range of techniques are expected to be applied in the studies of a material or class of High voltage normal versio n materials. Options for those who want to make their own Minimum version accessories and connections. It may also serve those who want to equip an earlier package with one or more Base unit system units to increase measurement throughput and make better use of all accessories. Custom systems A system designed specifically for your needs. NORECS AS
Standard ProboStat™ packages Example: Extensively furnished system package Typical use: System contains: Disk samples of varying diameters Ni-plated brass base unit 2, 3 and 4 electrode setups 2 outer tubes (alumina and silica) Van der Pauw 4-point measurements 3 alumina sample support tube assemblies Bar samples (4-point and Seebeck 2 alumina spring load assemblies coefficient measurements) 3 gas supply tubes (alumina and silica) Conductivity, impedance spectroscopy, 4 thermocouples (Pt/Pt10%Rh) DC measurements 15 Pt/alumina electrode connection assemblies Concentration cells; transport number, Pt net electrodes, Au seal rings, manual, permeability, fuel cell testing etc. storage case, stand and more. NORECS AS
Measurement setups Assembling the ProboStat™ for measurements is similar in all methods, with only minor replacement of accessories NORECS AS
Measurement setup; Disk sample Here we demonstrate setting-up of the simplest 2-point conductivity method with two electrode contact pairs from the outer chamber. E. Mount D. Connect an spring-force electrode C. Place sample assembly and contact pair for B. Connect an equipped with the outer gas the upper A. Mount inner electrode two centered supply tube. electrode. gas supply tube contact pair for electrodes. Attach control and sample the lower thermocouple. support tube . electrode. NORECS AS
Measurement setup; Disk sample Schematic illustration of assembly of disk sample measurements Setup 1 Setup 2 2-electrode conductivity & 2-electrode conductivity & impedance spectroscopy impedance spectroscopy using two outer electrode using inner and outer contacts electrode contacts Instead of using the outer 2-point conductivity method with two outer electrode connection for the “hand” electrode contacts lower electrode, you may use (only top part of the cell is the inner electrode shown). connection for 2-electrode conductivity measurements. Setup 2 is changed into the setup 3 by using gold gasket for sealing sample on the support tube edge. NORECS AS
Measurement setup; Disk sample Schematic illustration of assembly of disk sample measurements Setup 4 Setup 3 2- and 3-electrode 2-electrode conductivity & conductivity / impedance impedance spectroscopy, spectroscopy / voltammetry transport number with guard ring measurements by emf of concentration cell or fuel cell A guard electrode contact testing with seal used in the combination with the setup 2 may be used for For the concentration cell 2-point conductivity emf transport number measurements on disk measurements, or fuel cell sample with surface guard, testing: seal the setup 2 on electrode impedance the support tube edge. The studies with ring reference electrode – seal and the sample symmetrical cell, and voltammetry studies with separate the inner and outer ring reference electrode – symmetrical cell. gas compartments in the The guard electrode contact can also have cell. sealing function. NORECS AS
Measurement setup; Disk sample Schematic illustration of assembly of disk sample measurements Setup 5 Setup 6 Van der Pauw 4-point Permeability measurements conductivity for use with GS or MC measurements on disk sample In typical permeability experiment, a disk sample is The van der Pauw method requires specially sealed gas tight over the designed electrode support tube. contacts and two-rod spring-force assembly, but the basis of the setup is the same as for the above-listed setups. NORECS AS
Measurement setup; Disk sample Example: Fuel cell test (setup 3) P at 800 o C U at 800 o C P at 700 o C U at 700 o C 1,2 0,6 Fuel Cell: ASC2 anode: porous NiO/8YSZ 1,0 electrolyte: dense 8YSZ 0,4 cathode: porous LSCF P, W/cm 2 0,8 U, V Fuel: wet H 2 ; Oxidant: dry air; 0,6 0,2 Gas flow rate 30 ml/min. Sealing: SOFC test with the ProboStat™ 0,4 Gold gasket and FCMix – a simple gas mixer 0,0 OCV theor = 1.102 V for fuel cell research (University 0,2 OCV exp = 1.091 V of Oslo) 0,0 0,5 1,0 1,5 I, A/cm 2 Fuel cell performance for: wet H 2 , Pt I ASC2 I Pt, dry air NORECS AS
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