Metravib. Materials characterization at its best. 01dB-Metravib.

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1 AREVA is a worldwide expert in the energy field, with a strong industrial presence in over 40 countries. The group provides its clients with technological solutions for nuclear energy production, electricity transmission and distribution. AREVA also offers interconnect systems, principally in the telecommunications, computer and automotive markets. The 75,000 AREVA employees are thus committed to the major challenges of the 21st century : access to energy for everyone, preservation of the planet and responsibility towards future generations dB-Metravib Metravib Materials characterization at its best July Version 2006 O1dB-Metravib Siège Social FRANCE 200, Chemin des Ormeaux F Limonest Cedex Tél. : +33 (0) Fax. : +33 (0) Asia Pacific Tel. : Fax : Brazil Tel. : Fax : Germany Tel. : Fax : Italy Tel. : Fax : USA Tel. : Fax :

2 A range of mechanical analyzers meeting all your requirements Your materials Thermoplastic polymers Thermosetting polymers Elastomers Composites Adhesives Paints and varnishes Foods Cosmetics Pharmaceuticals Oils Biomaterials Glass and ceramics Metals and alloys... G' MetraviB 35 years experience and innovation 01dB-Metravib has been specializing in vibration engineering, reduction of noise, and vibration pollution since The company has combined its expertise in vibration mechanics with its need to characterize the physical properties of materials to develop innovating instruments for mechanical characterization. From the first viscoelasticimeters sold in 1972 to robotized systems (ROB0) for the mass characterization of specimens, 01dB-Metravib has always developed new analytical techniques meeting the expectations of both scientists and manufacturers. Your analytical needs Analysis of material intrinsic properties Young s modulus (E*), Shear modulus (G*), Tan δ Frequency behavior Temperature behavior Operating temperature range Glass transition (Tg) Melting Post curing phenomena Non-linear behavior of elastomers (Payne effect, Mullins effect) Creep/relaxation behavior tanδ Dynamic Mechanical Analysis the key to control the thermo-mechanical performances of materials Dynamic Mechanical Analysis consists of applying a vibration of known amplitude and frequency (off resonance frequency) to a material specimen. Measurements of the applied displacement and the resulting force lead to the precise determination of viscoelastic properties, the Young s modulus (E*), or shear modulus (G*), depending on the deformation mode. DMA+0/150/450 DMA tests, TMA tests and fatigue tests at imposed strain or stress with forces up to 0 N, 150 N or 450 N forces Comparative analysis of the mechanical properties of industrial parts Stiffness K, K, K Loss angle Stress/deformation relationship Analysis of (static) thermomechanical behavior Thermal dilatation Penetration Indentation Simultaneous analysis of material rheological properties during curing cycles Initial viscosity Minimum viscosity Gel time Curing time E* Dynamic Mechanical Analysis (DMA) is a major characterization technique used to control mechanical performances and the temperature behavior of materials. Possible applications are constantly being developed. MetraviB A unique selection of innovating, high performing, and upgradeable mechanical analyzers DMA 50 DMA tests, TMA tests at imposed strain or stress with forces up to 50 N Because requirements in research or industrial testing have broadened considerably 01dB-Metravib has developed products that can measure glass transition temperatures, follow-up of transformation processes, robotized characterization of viscoelastic properties of specimens, etc. Based on a great capacity for innovation and recognized expertise in structure calculation, vibration, and physical measurements of materials, 01dB-Metravib has developed a unique range of instruments meeting multiple requirements along two major axes: scientific research: to understand the relationships between the material s molecular structure and its mechanical properties, industry: to control the key performances of manufactured products in their conditions of use and ensure their manufacturing quality and lifetime ROB 0 Robotized DMA, TMA and fatigue tests on a large quantity of specimens VHF 4 Measurement of very high frequencies viscoelastic properties VHR 5 DMA tests in torsion mode Analysis of mechanical properties versus environmental conditions Humidity UV radiations Oxygen Resistance to solvents, fuels

3 DMA 50 : accurate, versatile & cost-effective DMA 50 is a desktop DMA offering a high force range and outstanding flexibility from glass transition determination to immersed tests, which makes it a thermomechanical testing platform. Main assets High force: 50 Newtons Broad frequency range: from 1E-5Hz to 200 Hz Broad temperature range: from -150 C to 600 C Analysis of specimens with sizes representative of the material High performance of the auto-tension mode (coupled static/dynamic control) for film and 3-points bending modes Multi-purpose thermal chamber Reversible frame Possible immersed tests for all stress modes at no extra cost Simple to use Can be used with simple electric power supply Low price Main uses DMA, TMA, simultaneous DMA/TMA tests with DYNATEST software Determination of glass and secondary transitions Particularly well suited to polymers and composites Analysis of films and specimens with small stiffnesses Tests on materials immersed in a liquid R&D / Quality control Education / Lab work Precise With its metrological selections, innovating dynamic, static control algorithms, DMA 50 guarantees optimum control of all parameters influencing measurement quality. High force DMA 50N includes a dedicated electrodynamic actuator (01dB-Metravib patent), specifically designed to meet DMA requirements. This gives DMA 50 a great flexibility regarding the material s change of mechanical behavior versus temperature, and the capacity to analyze specimens with sizes that are representative of material structure, for either dynamic tests or static tests (creep, TMA). Ergonomics The automatically opening/closing thermal chamber allows for large clearance and, free access to the specimen, as well as very comfortable handling conditions for the operator. Versatile and flexible Flexible operating modes allow for instant repeating of routine DMA and TMA tests, as well as for the definition of specific tests combining multiple parameter settings. Depending on the test configuration, the position of the mechanical frame can be easily reversed. For tests requiring the specimen to be immersed in liquid, this function is particularly effective, since it allows use of all the available specimen-holders, regardless of the stress mode and does not require the purchase of expensive accessories. Bending-mode test on a composite material immersed in a solvent bath Suited to each material A range of 8 specimen holders allows for different types of strain (tension, compression, bending and shear) for a great variety of materials of very diverse shapes: fibers, films, plates, cylinders, pasty materials, etc. Upgradeable DMA 50 allows for the set-up of an additional channel to facilitate analysis coupled with the DMA test. Acquisition of additional measurement channels is possible: temperature, hygrometry, oxygen, gas atmosphere, etc. Cost-effective DMA 50 is a cost-attractive platform for thermal and mechanical characterization. It can be used from a regular main outlet. For subambient working conditions, DMA50N can be coupled to either an oven-stabilized bath, or a cryogenic source. DMA 50 s productivity is enhanced by automatic test sequencing capabilities Compression plates Tension jaws for films Planar shear Extensible 3-points bending Tension jaws for bars Tension jaws for fibers Shear jaws for films Single/dual cantilever

4 DMA + 0 / DMA / DMA : The reference in electrodynamic testing DMA+0, DMA+150, DMA+450 have very rigid frames that exhibit ranges of measurable stiffness and frequency that are unrivalled on the market. The range of available specimen holders, along with DYNATEST and MULTIDYN analysis software, make it a new type of universal electrodynamic testing machine that goes beyond classic DMA products. Main assets Very rigid mechanical frame (more than servo-hydraulic machines) High force: 0, 150 or 450 Newtons Unique stiffness range: up to 7 decades can be used in a single test Unique frequency domain: from 1E-5Hz to00 Hz High measurement precision Analysis of specimens with material-representative size Main uses Simultaneous DMA & TMA tests using DYNATEST software Fatigue and controlled waveform tests using MULTIDYN software Precise measurement of viscoelastic properties Determination of glass transition and and secondary transitions Thermal chamber with high heating rate Displacement stroke up to 12 mm for creep and stress relaxation tests Broad selection of specimen holders for multiple geometries and dimensions Easily upgradeable to meet specific analytical requirements Reduced maintenance DMA+0N, et DMA+150 : particularly well suited to polymers and composites (polymer materials, polymerization follow-up, fatigue) DMA+450N : particularly well suited to elastomer testing and characterization (Mullins effect, Payne effect, frequency sweep, etc.) Analysis of solid, viscous, and liquid materials Based on a wide range of specimen holders, DMA+0, DMA+150, DMA+450 can analyze a large variety of materials and specimen dimensions. Selecting the appropriate specimen-holder allows the instrument to adapt to: various excitation modes (tension, compression, bending, shear) the material nature (solid, paste, liquid) various specimen dimensions (plates, cylinders, films, fibers, gels, foams, etc.) the expected state of the material during the analysis (glassy state, glass transition, rubbery state, hardening, fluidizing, melting, etc.) Great versatility and flexibility DMA+0, DMA+150 and DMA+450 include Metravib s software DYNATEST, which has been specifically developed to drive the instruments and perform data acquisition and processing. Many test modes are available to analyze viscoelastic material properties precisely, along with their dependence on many parameters (temperature, excitation frequency, strain, force, time, mechanical or thermal history, etc.) Furthermore, instant calculation of master curves, creep/stress relaxation tests, and TMA tests provide DMA+ with a unique flexibility. All-in-one DMA and fatigue machine MULTIDYN software can be used to control the waveform applied to the specimen and turn DMA+ into a fatigue machine, bringing it unique versatility. From elastomer to reinforced polymers, fatigue tests can be performed with virtually an unlimited number of cycles and testing time. Compression plates Tension jaws for films Planar shear Unique mechanical features and technological control The very high rigidity of mechanical frames is one of the key points of the DMA+ performances. The technologies used to generate the excitation signal, measure the displacement and force transferred to the specimen have been specifically developed by 01dB-Metravib engineers, experts in vibration mechanics, to provide the DMA+ range with the optimum performances required for a fine analysis of viscoelastic material properties. This allows DMA+ to carry out high-precision measurements of complex moduli and of Tan delta. 3-point bending Single/dual cantilever Shear for pasty materials Tension jaws for bars Tension jaws for fibers Shear jaws for films Shear for liquids

5 Applications of analyzers Measurement of glass transition and melting DMA is recognized as the most accurate technique to determine the glass transition temperature (Tg). The Tg measurement precision of MetraviB DMA results from many technical innovations and specificities: auto-calibration of the loss angle measurement, quality of the thermal control, control of test dynamic conditions... By convention, the analysis is commonly performed at 1 Hz. In the example opposite, a PET specimen was analyzed between tension/compression clamps. The test was then carried out at high temperature, which also allowed to determine the melting temperature. It has evidenced the unique capacity of DMA+ to characterize huge variations in mechanical properties: during the test, the module can vary by a factor! Tg : 82 C Melting : 128 C Measurement of secondary transitions The determination of these very small-amplitude phenomena (β and γ transitions) on the Tan delta curve yields information on the impact resistance performances of polymers. The broad stiffness analysis range and the measurement precision of MetraviB analyzers allow to perform this type of analysis in very diverse stress modes and geometries depending on the available materials. β : -18 C Tg : 48 C Frequency effect The excitation frequency can have a significant influence on the modulus and loss factor a polymer material. Also, the glass transition can change significantly depending on the excitation frequency. Characterizing the frequency dependence of the material behavior will then be all the more important as the material is dynamically stressed in its final use, in particular if it is used for a damping function in a vibratory environment. In the example opposite, an epoxy resin exhibits a Tg increase of 15 C for an excitation varying from Hz to Hz. Tg (0,1Hz) : 144,6 C Tg (Hz) : 155,8 C Optimization of a transformation process The polymer cross-linking reaction is characterized by the transition from pasty state to solid state, via a fluidizing phase, under the competing effects of the temperature and of the chemical reaction. The great rigidity of the DMA+ 150 frame and the auto-control mode of Dynatest allow for the constant monitoring of the shear modulus during a single test and for the determination of process-characteristic times: minimum viscosity, gel time, etc. Depending on the nature of the material (prepreg, resin, etc.), different specimen holders can be used to perform this type of test. In the example presented here, a thermosetting resin was analyzed in shear mode. Characteristic points, along with important variations of the modulus (-million factor!) during the test, were collected. Fluidizing Gelification Characterization of non-linear properties of elastomers Regardless of their formulation, elastomers follow complex behavior laws under static and dynamic stress. Due to an accurate control of the deformation ratio applied to a specimen and to an important excitation force, DMA+ 450 allows for the analysis over particularly broad ranges of deformation ratios: from % to 300%. Multiple parameter settings are available in Dynatest and can be used to simulate complex stress conditions very precisely and make DMA+ must-have tools for the dimensioning and optimization of the mechanical behavior of elastomer parts. Fatigue test Fatigue tests can be performed with the DMA+ range of instruments, using the Multidyn software. The test opposite shows the important decrease of the material s modulus after 0000 cycles and the evolution of its response through Lissajou curves. The test can be performed using a controlled waveform, which allows to reproduce specific test conditions that are representative of the material s final use. Characterization of materials ageing The comparative analysis of a new composite material and of the same material subjected to thermomechanical ageing has showed markedly different mechanical properties: glass transition temperature, damping and elastic modulus. In the example opposite, material ageing led to a 4-fold decrease of the elastic modulus and to a 40 C increase of the glass transition temperature, with a drastic loss of the damping factor (from 0.32 to 7). Immersion test The impact of water absorption on the mechanical properties of a polymer can be characterized by performing the test on a polymer specimen immersed in water. DMA 50 makes this test very simple. One just need to put the mechanical frame upside down and once the specimen is set into place, to immerse it into a bath. All specimen holders of DMA 50 can be used for this type of test. In the example opposite, one can note the instant fall of the modulus upon immersion, which continues until the specimen breaks up. Prediction of long-term creep Performing a few-minute creep test on different consecutive temperature plateaus has allowed, based on Dynatest TTS (Time Temperature Superposition) calculation, to predict the material s creep over several months or years. The creep test can be performed in stress modes, usually 3-point bending modes for highmodulus materials, but also, based on DMA+ performances (very rigid frame and high excitation force) using tension clamping jaws on specimens with significant geometry, in regards to material's structure. Immersion Test New material Aged material 1 year years

6 Main characteristics DMA 50 DMA+0 DMA+150 DMA+450 Maximum (+/-) Force (N) Minimum (+/-) Resolution (N) Displacement (µm) Frequency (Hz) Deformation modes Maximum (+/-) Minimum (+/-) 1 1 Resolution (nm) Minimum (Hz) 1E-5 1E-5 1E-5 Maximum (Hz) Maximum (Hz) (option) Resolution (%) points bending Single/double cantilever Tension Compression 1 3 1E MECHANICAL Characteristics Shear Temperature ( C) Minimum ( C) room room Minimum ( C) option Variation rate Maximum ( C) Maximum ( C) option 600 on request Minimum heating Maximum heating Minimum cooling Maximum cooling THERMAL Characteristics Stability ( C) Thermal control stability (+/-) Minimum (Pa) Modulus (Pa) Tan delta Maximum (Pa) 3E+12 3E+12 Measurement range (decades) MATERIALS Sensitivity Resolution dB-Metravib keeps right modify its intruments characteristics without prior notice. Additional information is available as technical notes and datasheets: DYNATEST DMA theoretical backgrounds MULTIDYN DMA 50 specimen-holders VHF 4 DMA+0/150/450 specimen-holders VHR 5 Application notes ROB 0 The reference in Dynamic Mechanical Analysis L OREAL - TOTALFINAELF - EUROCOPTER - EADS - FLEXSYS - ONERA - C.R.R. - FIAT - CITROEN Automobiles - HISPANO SUIZA - GOODYEAR Technical Center Luxembourg - GOODYEAR Research Center Akron - CNES - GEC ALSTHOM - SUMITOMO - RHODIA Silica - BRIDG RIDGESTONE - PEUGEOT Automobiles - DUPONT DE NEMOURS - E.D.F. - SAINT GOBAIN - L.R.C.C. C.C.P. - RENAULT - MAXXIS Tires - COLAS - GERLAND ROUTE - DGA - E.N.S.B.A.N.A. - E.N.S.M.P. - E.N.S.C.L. - MAPA - MARK IV Automotive - G.D.F. - MICHELIN Centre de Technologie de Ladoux - MICHELIN American Research Center - RIETER - MICHELIN Rubber Asia - HUTCHINSON - INSA Lyon - POLYFIBRON - HENKEL - ITT Automotive - REPSOL - Mac MASTER University - WOO - SUNG Tire - University of Delft - APOLLO Tires - JK Tires - Indian Rubber Manufacturers Asso - ciation - B.A.R.C. - TRELLEBORG - Beijing Research Institute of Materials and Technology - Institute of Materials of Moscow - University of Michigan - University of Cambridge - University of Sheffield - Université de Compiègne - Université d Orléans - Université de Savoie - Univer- More than instruments, SERVICES: With 01dB-Metravib, you benefit from: Specialists expertise to help you to purchase your analyzer Specialists expertise to help you to get familiar with DMA Inter-company training sessions Customized training sessions by specialists The guarantee to control the quality of your tests The guarantee to meet changes in your analytical needs A competent and reactive after-sales department Technical support (hotline) Access to customized tests services