Introduction

1.1 TMA

Thermo mechanical analysis (TMA) is a thermal analysis used in materials science where sample displacement, such as volume growth and shrinkage, is measured as a function of temperature, time, and applied force. It is one of the simplest techniques in thermal analysis usually used to characterize linear expansion, coefficient of thermal expansion (CTE), glass transitions (Tg), and softening points of materials [1, 2]. The figure below illustrates a typical TMA instrument.

Fig. 1 Schematic diagram of a simple TMA Apparatus [3]. This technique works by having a cylindrical or oblong sample, which sits on a furnace, subjected to slight loading via a probe made of a material with low, reproducible, accurately known CTE, and has low thermal conductivity. Load applied may be by static weights or by force motor. Probes are usually made of quartz glass and have different shapes to accommodate different sample geometries and specific experimental goals as illustrated in Fig. 2. It is important to use the right probe to get accurate results like for an accurate CTE; it is good to use a large probe area as well as low applied load. The probe senses the change in length by using a sensitive position transducer like a Linear Variable Displacement Transducer (LVDT) to measure the change in length. The system will be heated at a slow rate where a thermocouple near the sample measures the temperature and the probe moves according to the expansion or contraction of the sample specimen [3, 4].

Fig. 2 Different Probe shapes used in TMA: (1) Normal Probe, (2) Penetration Probe, (3) Macroprobe, (4) for Films/Fibers in the tensile mode [4]. In TMA measurement, the stages involved are: (1) preparing clean plane-parallel sample specimens, (2) measuring the initial length of the sample, (3) loading the sample in the instrument, (4) choosing the applied load, and (5) choosing the suitable experimental parameters. There are also factors that can influence the results of the experiment such as type of load, shape of probe, heating rate, starting temperature, sample geometry and preparation, and amount of load or stress applied [4]. Methodology TMA. The thermo mechanical analysis instrument used was TA Instruments TMA 2940. Furnace was in nitrogen environment with flow rate of 110 cm3/min and applied load was 0.50 N. For the first part, cylindrical brass and aluminium were used at heating rate 10oC/min. For the second part, different brass samples were used at different heating rates: 5oC/min, 7oC/min, and 10oC/min. For the data analysis, TA Universal Analysis was used and the CTE were found using the Alpha X1 to X2 analysis. Results and Discussion Thermomechanical Analysis The effects of heating rate on the TMA measurements were also observed by subjecting brass on different heating rates namely 5oC/min, 7oC/min and 10oC/min. The data gathered from TMA is illustrated at the figure below. The plots of the brass at different heating rates were very similar. The only slight difference is that the lower the heating rate, a flattened part is more observed. Other than that, there was not much of a significant difference found between the plots. Based from the plots, the CTE found were 20.16 m/(m.oC) for the 5oC/min heating rate, 22.58 m/(m.oC) for the 7oC/min heating rate, and 22.22 m/(m.oC) for the 10oC/min heating rate. There was not much of significant difference found in the CTE values found.

------ 5oC/min ------ 7oC/min ------ 10oC/min

Fig. # Brass Dimension Change vs Temperature at different Heating Rates It was observed in previous studies that heating rate have an effect on the penetration ramp rate of the probe on the sample. The higher the heating rate, the higher the penetration rate is that may have been due to the greater time for the refractory components to dissolve into the sample [Lucas 2001]. It was also found that the slower the heating rate, the longer the time available for recrystallizationn which explains the presence of the flattened parts of the plot [Lucas 2001]. The heating also has an effect on the Tg since as the heating rate is decreased, the deflection at Tg is increased [Slough]. Thermogravimetric Analysis Thermogravimetric graphs are often used to describe the chemical reactions that happen in a sample considering weight changes occur. A TGA curve of a white powder sample ceramic illustrated at the figure below shows that the sample undergoes a multi-step decomposition [Widman 2001].

Fig. # TGA curve of a Sample Ceramic The effect of weight on the TGA-DTA measurements were observed by analyzing a ceramic at two different weights, 152.1852mg and 145.6361mg, as shown at the figure below. From the plots, it can be observed that

------ 152.1852mg ------ 145.6361mg

Fig. # Percent Weight vs Temperature of a ceramic material at different weights

References [1] TMA Thermo Mechanical Analysis. (2013). Linseis Thermal Analysis. Retrieved August 20, 2013, from http://www.thermal-analysis.com/tma-thermo-mechanical-analysis.html [2] Menard, K. Thermomechanical Analysis Basics: Part 1 Its All Free Volume. Perkin Elemer Instruments. Retrieved August 20, 2013, from http://depts.washington.edu/mseuser/Equipment/RefNotes/TMA_Basics1.pdf [3] Introduction to Thermomechanical Analysis. Anasys Thermal Methods Consultancy. Retrieved August 22, 2013, from http://www.anasys.co.uk/library/tma1.htm [4] Thermomechanical Analysis. Retrieved August 20, 2013, from http://www.lkt.unierlangen.de/publikationen/buecher/Leseprobe_ptak-e.pdf [#] Lucas, J.A. (2001, March). Development of the Thermomechanical Analysis Technique for Coal Ash and Slag Applications Project 3.5 Final Report. Cooperative Research Centre for Black Coal Utilisation. Retrieved August 21, 2013, from http://www.ccsd.biz/publications/files/RR/RR18%20Dev%20of%20the%20thermomechanical.p df [#] Slough, C.G. Characteristic of Tg Detection Using Micro Thermomechanical Analysis. TA Instruments. Retrieved August 22, 2013, from www.tainstruments.com%2Flibrary_download.aspx%3Ffile%3DTA277.pdf

[#] Widman, G. (2001, January). Interpreting TGA curves. UserCom. Retrieved August 22, 2013, from http://www.masontechnology.ie/x/Usercom_13.pdf [#]