The Flash DSC 1 A Novel Rapid Scanning Calorimeter

Transcription

1 The Flash DSC 1 A Novel Rapid Scanning Calorimeter Hay Berden Mettler-Toledo B.V. Tiel. Version 1.0. July, 2010 Author: J. Schawe Review: A. Hammer

2 Contents Who is Mettler-Toledo The DSC Technique - Conventional DSC Curve of PET Reorganization During the Measurement The Flash DSC 1 - The Chip Sensor DSC of Metastable Materials Flash DSC Basics - Typical Experiment - Variation of Heating Rates - Variation of Cooling Rates - Isothermal Experiment Application Areas of the Flash DSC 1 Applications Summary 1

3 Our Group METTLER TOLEDO is a global manufacturer and marketer of precision instruments for use in the laboratories, manufacturing, and food retailing. <Worldwide presence < employees <Sales approx. msd

4 Group Sales in musd

5 Sales per Region in musd Americas 35% Europe 41% Asia / RoW 24%

6 Strongest Brand 5

7 Global Manufacturing, Sales & Service Innovation Centers MT Sales & Service Organizations MT Partners Global manufacturing strategy with focused innovation centers Approx employees in sales & service in 35 countries 6

8 Customer Processes Solutions to support customer processes R&D Drug Discovery Quality Control Logistics Retail Manufacturing Packaging Laboratory Solutions Industrial Solutions Retail Solutions Customer Benefits <Accelerate processes <Improve product quality 7 <Increase efficiency <Comply with regulations

9 Advancing Research and Quality Control Laboratory Solutions Improving processes in R&D, drug discovery and quality control Application-specific software Interface with your information systems Enhanced accuracy, productivity and compliance Laboratory Weighing Solutions Laboratory Balances Pipettes Analytical Chemistry Thermal Analysis Automated Chemistry Solutions 8

10 Improving Productivity Industrial Solutions Optimizing your operations from receiving to shipping Improved product quality Accelerated and automated processes & ERP integration Increased efficiency Regulatory compliance Receiving Process Analytics Industrial Weighing End-of-Line Product Inspection Logistics 9

11 Optimizing Fresh Foods Management Retail Solutions Effectively manage your fresh foods inventory and merchandising Maximize your efficiency and profitability Enhance the satisfaction of your customers Integrated in existing IT infrastructures Central Pack Receiving Prepack Counter Self-Service Checkout 10

12 Innovation Competencies Man / Machine Interface In Process Technology Technology Integration Customer Applications Automation & Robotics 830 R&D professionals work daily on maintaining our technology lead 11

13 Service Solutions Service XXL Customer Benefits Validatiodation Vali- Support Regulatory Qualification Compliance Calibration Validation methods and protocols ensure process reproducibility, user monitoring and safe data management. Documented equipment qualification ensures compliance with quality assurance systems such as GLP, GMP and ISO. Calibration processes ensure accurate, reliable and traceable results. Maintenance and Support Proactive maintenance maximizes uptime and productivity. User training ensures equipment knowledge which leads to safer working processes. Improved service tools enhance customer processes 12

14 The Success Story of Thermal Analysis Dr Erhard Mettler In 1945, a Swiss engineer named Dr Erhard Mettler started a precision mechanics company near Zurich, Switzerland. The «Mettler balance» became a synonym for the lab balance. The analytical balance from 1945 Dr Hans-Georg Wiedemann In the early 1960s, Dr Wiedemann convinced Dr Mettler to combine the advanced weighing technology with a furnace. This lead to the introduction of the TA1. The TA1 from 1964 The first TGA/DTA 13

15 The Success Story of Thermal Analysis Substitution balance (1940s) Modular concept (1960s) Multi-pile TGA-DSC sensor (1970s) Microprocessorcontrolled system (1980s) Automation (1990s) DMA with high frequencies (2002) Flash DSC 1 (2010) Thermal Analysis Excellence (2007) TOPEM TMDSC (2005) MultiSTAR DSC sensors (2004) Innovation since

16 Thermal Analysis Excellence Innovative Technology Versatile Modularity Swiss Quality 15

17 Overview on Thermal Analysis: Video The Future of Thermal Analysis Innovative Technology Versatile Modularity Swiss Quality Click to watch the video 16

18 The DSC Technique Conventional DSC Measuring Principle Sample Heat flow Reference Typical experimental conditions: Sample weight: 1 20 mg Heating rate: K/min Measured property: Heat flow 17

19 Innovative Technology Flash DSC 1: A Quantum Leap in Innovation Opens up New Frontiers } Heart of the Flash DSC 1 is the chip sensor based on MEMS technology MEMS: Micro-Electro-Mechanical Systems 18

20 The DSC Technique: DSC Curve of PET 19

21 Reorganization During the Measurement 20

22 The Flash DSC 1 Heating rates up to K/min Cooling rates up to K/min Overlap with conventional DSC Simple sample preparation Measures from -95 C 450 C The DSC 1 and the Flash DSC 1 together cover a scanning rate range of more than 7 decades. 21

23 The Flash DSC 1 Easy sample preparation and sensor change thanks to the ergonomic design. 22

24 The Flash DSC 1: The Chip Sensor Ceramic plate Silicon frame Bonding wire Thermocouple Aluminum plate Resistance heater The MultiSTAR UFS 1 chip sensor is a DSC sensor based on MEMS technology (Micro-Electro-Mechanical Systems). The sensor consists of two identical silicon-nitride/oxide membranes, 1.6 mm 1.6 mm, 2 μm thick, mounted in a silicon frame, 300 μm thick. 23

25 The Flash DSC 1: The Chip Sensor 1 The sample area is 0.5 mm in diameter and coated with aluminum to achieve a homogeneous temperature distribution. Eight thermocouples measure the temperature on each side. 24

26 Metastable Materials Polymers Polymorphic substances Many blends and alloys Many composites The structure of such materials depends on the cooling conditions used when they were prepared or produced. On heating, reorganization can occur. This is the reason why the conventional DSC curve does not always correspond to the structure of the original sample. 25

27 Flash DSC Basics: A Typical Experiment Sample preparation Formation of sample structure Analysis Melting of the sample optimizes thermal contact. Different cooling rates allow defined sample structures to be formed. High heating rates suppress the reorganization of the sample. Itcan therefore be measured as received. 26

28 Flash DSC Basics: Variation of Heating Rate Examples of reorganization processes: Separation or elimination of phases Melting of unstable crystallites with formation of more stable crystals Transitions of polymorphic phases Reorganization is often determined by kinetic processes and is therefore time dependent. The possible influence of reorganization on the heating curve can be detected by varying the heating rate of the Flash DSC 1 over a wide range. 27

29 Flash DSC Basics: Variation of Cooling Rate The formation of structure can be investigated by performing measurements at different cooling rates. In particular, technical processes carried out at high cooling rates can be simulated in the Flash DSC 1. Information is obtained about the effect of additives such as nucleating agents under near-process conditions. Spritzgussform für LEGO Steine Quelle: Injection molding equipment Source: LEGO Systems, Inc. 28

30 Flash DSC Basics: Isothermal Experiment Isothermal measurements provide detailed and direct information on the kinetics of fast transitions and reactions that take place in a few seconds. The high cooling rates and accurate temperature control often allow materials to be cooled from the melt to the crystallization temperature without undesired formation of structure. 29

31 Application areas of the Flash DSC 1 Detailed analysis of structure formation processes in materials. Direct measurement of fast crystallization processes Determination of the reaction kinetics of fast reactions Investigation of the mechanism of action of additives under nearproduction conditions Comprehensive thermal analysis of materials in a very short time Analysis of very small amounts of sample Determination of technical data for simulation calculations 30

32 Flash DSC Applications 1 Calibration substances 31

33 Flash DSC Applications 2 Melting of PET 32

34 Flash DSC Applications 2 Melting of PET 33

35 Flash DSC Applications 3 Reorganization of ipp 34

36 Flash DSC Applications 4 Isothermal crystallization 35

37 Flash DSC Applications 4 Isothermal crystallization 36

38 Flash DSC Applications 5 Nanofiller in PA 11 37

39 Flash DSC Applications 6 Melting and decomposition Kurve mit 10 K/min löschen 38

40 Flash DSC Applications 7 Polymorphism 39

41 Summary The Flash DSC 1 is the ideal complement to conventional DSC for the characterization of modern materials and optimization of production processes. Fast and variable measurements save time in the analysis and development of materials. The quality of products can be improved through knowledge of structure formation under actual process cooling conditions. This data can be used to optimize processing conditions, molds, and tools. 40

42 Summary Features and Benefits of the Flash DSC 1 Ultra-high cooling rates allow materials with defined structural properties to be prepared Ultra-high heating rates reduce measurement times and suppress reorganization processes Fast-response sensor enables the kinetics of extremely fast reactions or crystallization processes to be studied High sensitivity low heating rates can also be used; scan rates overlap with those of conventional DSC Wide temperature range measurements can be performed in the range -95 to 450 C User-friendly ergonomics and functionality sample preparation is quick and easy 41

43 For More Information News Handbooks Webinars Thermal analysis in general 42

44 Thank You