购买
下载掌阅APP,畅读海量书库
立即打开
畅读海量书库
扫码下载掌阅APP

1. 4 Introduction to measurements

1. 4. 1 Scanning electron microscopy

The morphology of the polymer nanoparticles was analyzed via a scanning electron microscopy (SEM) (Cambridge, Leica) with an accelerating voltage value equal to 15 kV. The samples, analyzed in their cross section, were coated with a thin gold layer by means of a sputter coating (Polaron, model SC502 sputter coater) [21].

1. 4. 2 Differential scanning calorimetry (DSC)

DSC is one of the most convenient approaches to throw light on the degree of crystallinity along with the thermal behavior of any polymeric samples [4].The glass transition temperature (T g ) of the resulting polymer film was determined via DSC measurement. The T g of a polymer indicates the transition from a rubbery into a glassy state. Therefore, the polymer is flexible above the T g and hard and brittle below the T g [21].

In our study, DSC analysis was carried out with a Mettler Differential Scanning Calorimeter instrument (Figure 1. 5. ) under argon purge atmosphere flow (70. 0 mL/ min) [75] between -100 ℃ and 150 ℃ along with liquid nitrogen as a cooling element [34]. Samples around 5 ~ 7mg were sealed in 40 μL aluminum pans with perforated lids to allow the release and removal of the decomposition products [20]. Two segments of DSC scanning included:1)-100 ℃ isothermal for 10. 0 min, 2) with a heating rate of 10 ℃ / min and the temperature range from -100 to 150 ℃ . Another empty aluminum pan was placed as a reference.

Figure 1. 5. A schematic of DSC experiment

1. 4. 3 Thermogravimetric analysis

The thermal stability of the polymer electrolytes was measured by thermogravimetric analysis (TGA). Thermogravimetric measurement was carried out with a TGA/ SDTA851e thermal analyzer. Around 5. 442 mg of sample were placed in a TGA aluminum pan. The sample was heated from 25 ℃ to 130 ℃for 15 minutes and cooled rapidly to 25 ℃ for 15 min. Then the samples were heated up to 400℃ at a rate of 10 ℃ / min [12]. The fully amorphous nature of the polymer was observed under thermal characterization.

1. 4. 4 Cyclic voltammetry

The electrochemical stabilities of the SPE membranes were determined by cyclic voltammetry (CV) using a potentiostat / galvanostat (Solartron impedance analyzer). A testing cell was assembled to determine the oxidation potential with stainless steel as working electrode and lithium foil serving as a counter and reference electrode. All the scans were made at 25 ℃ at a scan rate of 10 mV/ s within a voltage range of 0 V to 5. 0 V versus Li / Li [76].

1. 4. 5 Ionic conductivity

The ionic conductivity of the obtained compounds was measured by the complex impedance method using an impedance analyzer (Solartron model SI1287; Schlumberger) coupled to a Solartron model-1260 frequency response analyzer. The membranes were sandwiched between two stainless steel electrodes of 2. 54 cm 2 in the area for conductivity measurement [77]. All the measurement was performed in a glove box filled with a dry nitrogen gas in a temperature range of 25 -70 ℃ [78].

The ionic conductivity (δ, in S cm - 1 ) was plagiaristic from the value of resistance (R, in Ω) of the bulk electrolyte obtained in the complex impedance diagram, in relation to the equation: δ = L/ (RS), where L (cm) is the thickness of the membrane of the polymer electrolyte, and S (cm 2 ) is the area of the membrane [22]. IMk/GbW0z3nXPKLdPujnBOIKIL/gRzc8V+jaJTsaPS0Gc36KpSGTQoo9hUydI7oo

点击中间区域
呼出菜单
上一章
目录
下一章
×