塑料.快速差示扫描量热法（FSC）.芯片量热法

[中文适用范围]： 本文件规定了非绝热快速差示扫描量热计的特性，也包含在具有开放样本几何形状的通用缩写 FSC 中，其中样本直接放置在基于微机电系统 (MEMS) 的芯片传感器的有源测量区域上膜技术，无需封装在封闭的坩埚和烘箱中。 由于样品几何形状开放，本文件仅适用于质量不大于 1 µg 的非常小的样品。 通过保持样品厚度尽可能小，可以防止测量过程中出现高温梯度。 使用非常低的样本质量可以在加热和冷却模式下实现数千 K/s 的非常高的扫描速率，从而较低的样本质量和厚度允许更高的加热和冷却速率。 通常，FSC 的低扫描速率与 ISO 11357-1 涵盖的传统 DSC 的高扫描速率重叠，从而能够连接到传统 DSC 结果。 注 1：由于传感器布局，FSC 也称为芯片量热法。 注 2：FSC 代表快速扫描量热法，也代表快速扫描量热仪。 在实践中，根据上下文可以很容易地做出选择。 FSC 适用于聚合物、聚合物共混物和复合材料的快速动力学效应的热分析，例如： ——热塑性塑料（聚合物、模塑料和其他模塑料，有或没有填料、纤维或增强材料）； ——热固性材料（未固化或固化材料，有或没有填料、纤维或增强材料）； ——弹性体（有或没有填料、纤维或增强材料）。 本文件规定了对显示热流率变化的快速物理和化学过程进行定性和定量分析的方法。 这包括测量固体和液体材料的特征温度以及热量值。 本文件特别适用于观察热效应的快速动力学，例如： - 物理转变（玻璃化转变、相变，例如熔化和结晶、多晶型转变等）； ——亚稳态和相关过程，如重组、（再）结晶、退火、老化、非晶化； ——化学反应（弹性体和热固性材料的水合、氧化、聚合、交联和固化、分解等）； ——快速结晶系统或化学反应的等温测量。 它还适用于热容和热力学函数相关变化的测定。 FSC 提供了一种技术来分析工业聚合物加工中使用的类似高加热或冷却速率下的材料行为。  1  FSC 还可以分离具有不同动力学的重叠热效应，例如： ——熔化和分解：较高的加热速率可以将分解转移到更高的温度，并允许不受干扰地测量熔化； ——聚合物的玻璃化转变和冷结晶：较高的加热速率可以抑制冷结晶，从而不受干扰地测量作为冷却/加热速率函数的玻璃化转变； ——无定形或半结晶聚合物在冷却和加热时的重组：根据所使用的冷却速率，可以生成具有不同结晶度的样品，并使用不同的扫描速率分析它们在加热时的重组。 本文件规定了 FSC 的一般方面，例如原理和设备、取样、校准以及程序和测试报告的一般方面。 [外文原描述]： This document specifies the characteristics of non-adiabatic fast differential scanning calorimeters, also covered by the general abbreviation FSC having an open specimen geometry in which specimens are placed directly onto active measurement areas of chip sensors based on Micro-Electro-Mechanical Systems (MEMS) membrane technology, without encapsulation in closed crucibles and ovens. Due to the open specimen geometry, this document is applicable to very small specimens having masses of not greater than 1 µg only. The occurrence of high temperature gradients during measurements can be prevented by keeping specimen thicknesses as small as possible. The use of very low specimen masses enables achievement of very high scanning rates in the order of several thousand K/s, both in heating and cooling mode whereby lower specimen masses and thicknesses allow higher heating and cooling rates. Typically, low scanning rates of FSC overlap with high scanning rates of conventional DSC covered by ISO 11357‑1, thus enabling connection to conventional DSC results. NOTE 1 Due to the sensor layout FSC is also called chip calorimetry. NOTE 2 FSC stands for Fast Scanning Calorimetry but also for Fast Scanning Calorimeter. In practice from the context the choice can be made quite easily. FSC is suitable for thermal analysis of fast kinetic effects of polymers, polymer blends and composites, such as: — thermoplastics (polymers, moulding compounds and other moulding materials, with or without fillers, fibres or reinforcements); — thermosets (uncured or cured materials, with or without fillers, fibres or reinforcements); — elastomers (with or without fillers, fibres or reinforcements). This document specifies methods for qualitative and quantitative analysis of fast physical and chemical processes showing changes in heat flow rate. This includes measurement of characteristic temperatures as well as caloric values of both, solid and liquid materials. This document is particularly applicable for the observation of fast kinetics of thermal effects such as: — physical transitions (glass transition, phase transitions such as melting and crystallization, polymorphic transitions, etc.); — metastability and related processes like reorganization, (re)crystallization, annealing, ageing, amorphization; — chemical reactions (hydration, oxidation, polymerisation, crosslinking and curing of elastomers and thermosets, decomposition, etc.); — isothermal measurements of fast crystallising systems or chemical reactions. It is also applicable for the determination of heat capacity and related changes of thermodynamic functions. FSC provides a technique to analyse material behaviour at similarly high heating or cooling rates used in industrial polymer processing. FSC can also enable separation of overlapping thermal effects with different kinetics such as: — melting and decomposition: higher heating rates can shift decomposition to higher temperatures and allow unperturbed measurement of melting; — glass transition and cold crystallisation of polymers: higher heating rates can suppress cold crystallisation resulting in unperturbed measurement of glass transition as a function of cooling / heating rates; — reorganisation of amorphous or semi-crystalline polymers upon cooling and heating: depending on the cooling rate used specimens with different crystallinities can be generated and their reorganisation upon heating analysed using different scanning rates. This document establishes general aspects of FSC, such as the principle and the apparatus, sampling, calibration and general aspects of the procedure and test report.