Isothermal Battery Calorimetry Method, Instrumentation and Application

ISOTHERMAL CALORIMETRY A Crucial Tool for Thermal Management of Battery Packs The success of electric-driven vehicles (EDVs) relies on the lithium-ion battery technology. While the battery manufacturers strive to develop more compact and powerful battery packs for EVDs, thermal management continues to be a major challenge because temper-ature is critical to battery performance, life, and safety. Numerous high profile accidents in recent years have exemplified this challenge. The IBC 284 is the testing equipment of choice when it comes to study high power and large battery packs for application in electric drive vehicles or airplanes. It was co-developed by the National Renewable Energy Laboratory (NREL, Golden, Colorado, USA), one of the leading research organizations in the development of analytical tools for designing optimized battery thermal management systems, and NETZSCH. The information gained from IBC 284 enables engineers to identify and classify materials and configurations suitable for advanced battery thermal management systems already in the early development stage and thus to reduce time to market.

Heat-transfer fluid Cut-away of the IBC 284 Calorimetry is the science of measuring the heat of chemical reactions or physical changes of a specimen. Depending on the transition or reaction of interest, the heat may be generated (exothermal process), consumed (endothermal process) or just dissipated by the sample which is applied to a controlled temperature profile.
For measuring inhomogeneous samples such as entire EVD battery packs, isothermal calorimetry, i.e., calorimetry at a defined constant temperature, is ideal. The isothermal temperature regime additionally simplifies the kinetics within the results.
The IBC 284 consists of a large volume analysis chamber, submerged in an isothermal bath. In contrast to air cooling systems, liquid heat-transfer fluids feature a much better temperature stability than gaseous media. In the IBC 284, a glycol-water mixture is used to reach also sub-ambient temperatures. Heat-flux gauges embedded in the bottom of the analysis chamber detect the heat released by the battery sample.
For cycling experiments, a commercial battery tester can be employed to charge and discharge the battery pack.

R&D AWARD WINNER IN 2013 The IBC 284 was winning the renowned R&D 100 award in 2013. This award, also sometimes called "Oscar of Innovation", dignifies the most sophisticated high-tech products of each year.
Various Safety Measures: The IBC 284 is ergonomically Slight Overpressure in the Analysis Chamber designed for a single operator to quickly set up and run numerous In order to avoid intrusion of the heat-transfer fluid into testing scenarios. The liquid level is the analysis chamber, the chamber is slightly pressurized conveniently controlled for sample with nitrogen, air or argon (automated dedicated loading and unloading. Large gauge, low-resistance cabling is secured into the design for easy connection to an external battery cycler system.
In case of battery thermal runaway, the burst disk will rupture and relieve the pressure inside the test chamber to maintain safety and protect the analysis chamber from damage.

For Various Kinds of Batteries The IBC 284 measures heat signatures of large format cells, but is also able to test smaller cylindrical, pouch and Reduced Time-to-Market prismatic cells.
Calorimetric-driven development can dramatically shorten the R&D period. Smart Concept for True Battery Heat Measurements Several design features, including an optimized heat-flux gauge location, routing the power cables through the isothermal bath and the attachment of the high-power connections to the test chamber, are introduced to eliminate heat losses.
Independent Determination of Charging and Discharging Efficiency The IBC offers the possibility to charac-terize the efficiency of batteries over different temperature ranges and states of charge (SOCs) with high accuracy. The IBC 284 is devised for accurate heat measurements, resulting in a better thermal management, improved performance, lifetime and safety of battery systems.

The IBC 284 is the isothermal battery calorimeter for large battery packs. It has several unique, innovative features that allow it to be very accurate even with large batteries. These features include: ∙Total Thermal Insulation through ∙ Real World Temperature Range The IBC 284 operates from -30°C to The battery test chamber is completely +60°C covering the battery-pack testing submerged in an isothermal bath with range for all climates in accordance with very tight temperature control so that the the United States Advanced Battery ambient temperatures do not influence the Consortium (USABC) guidelines. heat-flux measurements. ∙Control Software for Turnkey Operation High Sensitivity Detection The IBC 284's optimized control software Heat-flux gauges can measure small can be pre-programmed to run a user quantities of heat energy flowing to/ defined temperature and stabilize before from the isothermal bath surrounding starting the charge or discharge test. the analysis chamber. Ergonomic design allows for fast test set-up and easy operation.
One Instrument for Various Battery Sizes The size of the IBC 284's analysis chamber allows cells and modules of different sizes to be tested – from large vehicles batteries with a feed size of 12x8x6 inches (30x20x15 cm) to small 18650 cells which are placed centered at the bottom of the chamber. Innovative Heat Retention Batteries for hybride electric vehicles (HEV), plug-in-hybride electric vehicles (PHEV) and electric vehicles (EV) can produce currents over 300 amps; large copper conductors are therefore required to safely carry these currents. Since these high-thermal-conduc-tivity copper cables are connected to battery terminals, they can conduct heat directly out of the calorimeter. This means (according to an NREL study) that up to 30% of the heat generated in the battery does not get measured by the heat-flux gauges. The IBC 284 is the only commercial calorimeter in the world that addresses this problem – it features heat-sinking busbars and cables routed though the isothermal bath. DATA YOU CAN TRUST Technical Specifications of the Calorimeter 12 x 8 x 6 (inches) Maximum battery size 30 x 20 x 15 (cm) Maximum power (heat 50 W Sensitivity 30 mW Temperature range -30°C to 60°C Baseline noise 5 mW Data acquistion rate 10 to 20 Hz Heating/cooling 5°C/hr Isothermal bath (temperature ±0.01°C Enthalpy accuracy ±2% Third party cycler Turn-key solution available DependentCharge/discharge current: up to 300 A Specification typical cycler Current accuracy: 5 mA Voltage accuracy: 1 mVCharge/discharge volts: 50 V 5% FS (0 to 10 psi transducer) Pressure accuracy (0 to 70 kPa) Intelligent Software Solutions The IBC measurement software, specifically tailored to large battery testing and the sophisticated and user-friendly NETZSCH Proteus® analysis software form a powerful set of tools. Running under the operation systems Windows™ 7 and Windows™ 8, this combination offers a wide range of essential routines. Amongst others, the following features can be found: ∙Easy set-up with online ∙All measured signals plotted in ∙Easy access to calibration files ∙Individual plot of multiple temperatures (based on the various thermocouples), voltages and currents ∙Plot of the measured heat-flux ∙Heat correction based on busbar ∙Enthalpy calculation ∙Calculation of the electrical power (calculation based on the measured voltage and current) ∙Integration of the electrical power to get the total power ∙Calculation and integration of ∙Calculating efficiency by comparing heat losses to electrical power ∙Plotting efficiency as a function of current or temperature The two screen shots show the user interfaces for temperature control and data acquisition.
Many car manufacturers facing the Corporate Average Fuel Economy (CAFE) standards in the US (54.5 miles per gallon by 2025) or the mandatory CO emission reductions targets for passenger cars (95 g/km by 2021) set Heat Output of a Pouch Cell by the European Union are looking at electric-drive strategies. Batteries that power these cars need to be affordable, high-performing, long-lasting, and operate at maximum efficiency in a wide range of driving conditions and climates. But inadequate and inaccurate knowledge of batteries' thermal properties can negatively affect lifespan, safety and costs.
Influencing Factors for Battery Life Time Geographic Impact on Battery Life (Data from NREL) Thermal Design Impact on Battery Life (Data from NREL) As illustrated in the figure below, a battery pack in a PHEV20* without cooling in a hot climate (like in Phoenix/Arizona) can last 7 years while the same battery could last almost 15 years in a cooler climate (like in Minne-apolis/Minnesota), if a drop down of the relative capacity to approx. 82% is taken as a criterion. An analog effect can be achieved by increasing the cooling efficiency.
The IBC 284's accurate measurement of batteries' thermal performance under various electrical loads and boundary conditions makes it possible for battery system engineers to design effective management systems. * PHEV = plug-in hybrid electric vehicle Heat Output of a Pouch Cell The IBC is able to provide critical heat generation and efficiency data for a battery under charge/discharge conditions. In the past, battery manufacturers could only estimate the round-trip efficiency of a battery through electrical measurements. The IBC 284, however, measures the heat directly. Therefore, it becomes possible to determine the loss mechanisms and thus the battery efficiency for both charge and discharge currents independently. Here, a series of tests was conducted on a single pouch cell (15Ah) to measure the heat output at different operating temperatures. A standard CC/CV (constant current/constant voltage) protocol – from 2.5 V to 4.15 V at 1C** until the current dropped down to 750 mA – was used for all tests. A single example of a charge and discharge cycle, which was Above: Examplary measurement of a pouch cell at 20°C; depicted are the heat-flux signal in blue, the power signal in green and the performed at 20°C, is shown in the temperature of the isothermal bath in red. left figure on the right. When the battery is cycled at 40°C, the heat generated by the cell and the Joule heating represents 2.37% (= 100% - 97.63%) of the total energy supplied by the battery (discharge efficiency). At 0°C, it is 10.84% of the total energy. This proves that the IBC 284 is sensitive to measure low level differences at heat rate generation as well as peak heating which varies widely depending on whether the battery is tested at 0°C, 20°C or 40°C.
The right graph highlights the temperature-dependent behavior of the battery. In terms of efficiency, the difference between 0°C and 40°C is lower than what is measured during a discharge; the charge efficiency Discharge efficiency Charge efficiency just increases from 94.69% at 0°C to 98.72% at 40°C. ** 1C refers to the discharge within 1 hour Temperature-dependence of charge/discharge efficiency Entropic Cell Studies During charging/discharging, heat in a cell is important.  A low charge or discharge rate reduces the produced by both the resistance of the various contribution of the non-reversible heat and reduces cell components (Joule heating) and the entropic the heat gradient within the cell. In the example below, reactions which are the exothermic or endothermic three fully charged cells, with varying chemistries, were reactions within the cell due to the transfer of ions discharged at constant current at a rate of C/10 (1 C and electrons. The IBC 284 will provide information refers to the discharge within 1 hour). Entropic studies about heat generation as a function of depth of identify regions of the discharge curve where cells are discharge (DOD). This information can help under- highly resistive – as an example, Cell C has very high stand cell performance. impedance below a depth of discharge of 80%.  Such studies can provide an understanding on how to These entropic studies are normally conducted at low improve efficiency and lifetime as a function of charge rates, and low heat output, so high sensitivity is Noramlized Heat Rate (mW/Ah) Depth of Dischange (%) Entropic Cell Studies – C/10 Constant Discharge of Three Different Cells at 30°C (Data from NREL) Expertise in Service All over the world, the name NETZSCH stands for comprehensive ∙Installation and commissioning support and expert, reliable service, before and after sale. Our qualified personnel from the technical service and application departments are ∙Hotline service always available for consultation. ∙Preventive maintenance ∙Individual maintenance services In special training programs tailored for you and your employees, you ∙Calibration service will learn to tap the full potential of your instrument. To maintain and ∙On-site repairs with emergency protect your investment, you will be accompanied by our experienced service for NETZSCH components service team over the entire life span of your instrument. ∙PC supported diagnostics ∙E-mail reporting The NETZSCH applications laboratories are a proficient partner for ∙Moving / exchange service nearly any Thermal Analysis issue. You will receive high-precision ∙Technical information service measurement results and valuable interpretations from us in the ∙Spare parts assistance shortest possible time. This will enable you to precisely characterize ∙Accessories catalogue new materials and components before actual installation, minimize ∙Software update service risks of failure, and gain decisive advantages over your competitors. For ∙Application support production problems, we can work with you to analyze concerns and ∙Environmental instrument recycling develop solutions. Comprehensive Solution Provider for Battery Design and Testing NETZSCH offers a broad variety of techniques for determining thermal properties such as heat capacity, thermal conductivity and thermal expansion. When combined with thermodynamic and kinetic infor-mation from calorimetry, these methods provide the means for designing thermal models for batteries. This in turn allows one to explore the many different aspects of battery research, such as material optimization, reliability, safety analysis and long-term stability. Differential Scanning Calorimetry (DSC) DSC/TGA-Mass Spec TMA, DMA, DSC, TGA, DEA Thermal Expansion Thermal Conductivity Battery Safety and Research Instruments Differential Scanning Calorimetry Simultaneous Thermal Analysis Five different instruments Four different instruments ∙Safety screening ∙Oxidation of anode Melting of separators ∙Cathode decomposition ∙SEi (solid-electrolyte interface) decomposition Multiple Mode Calorimetry Adiabatic Calorimetry Modular instrument Three different instruments ∙Thermal testing of ∙PTC (positive thermal Compatibility (cathode coefficient), CID (circuit materials, electrolytes) interrupt device), ∙Thermal management data Laser Flash Analysis Isothermal Battery Calorimetry Three different instruments for determination of ∙Large batteries and packs Thermal diffusivity ∙Thermal management Thermal conductivity "Jelly-roll" thermal ∙Maximum performance transport (jelly-roll = safety and lifetime design principle of cylindrical recharge- able batteries) The NETZSCH Group is a mid-sized, family-owned German company engaging in the manufacture of machinery and instrumentation with worldwide production, sales, and service branches.
The three Business Units – Analyzing & Testing, Grinding & Dispersing and Pumps & Systems – provide tailored solutions for highest-level needs. Over 3,000 employees at 210 sales and production centers in 35 countries across the globe guarantee that expert service is never far from our customers.
When it comes to Thermal Analysis, Calorimetry (adiabatic & reaction) and the determination of Thermophysical Properties, NETZSCH has it covered. Our 50 years of applications experience, broad state-of-the-art product line and comprehensive service offerings ensure that our solutions will not only meet your every requirement but also exceed your every expectation.
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Research Article Pharmacovigilance and drug safety in Calabria (Italy): 2012 adverse events analysis Chiara Giofrè, Francesca Scicchitano, Caterina Palleria, Carmela Mazzitello, Miriam Ciriaco, Luca Gallelli, Laura Paletta, Giuseppina Marrazzo, Christian Leporini, Pasquale Ventrice, Claudia Carbone, Patanè, Stefania Esposito, Felisa Cilurzo, Orietta Staltari, Emilio Russo, Giovambattista De Sarro, and the UNIVIGIL CZ GroupDepartment of Science of Health, School of Medicine, University of Catanzaro, Italy and Pharmacovigilance's Centre Calabria Region, University Hospital Mater Domini, Catanzaro, Italy


Draft 2014Activity Document OctOber 2013 International Life Sciences Institute TABLE OF CONTENTS Draft 2014 Activity Document – October 2013 Draft 2014 Activity Document – October 2013 Foreword Draft 2014 Activity Document – October 2013 FOREWORD BY THE EXECUTIVE AND SCIENTIFIC DIRECTOR