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In thermogravimetric analysis (TGA), a sample is continually weighted while heating, as an inert gas atmosphere is passed over it. Many solids undergo reactions that evolve gaseous byproducts. In TGA, these gaseous byproducts are removed and changes in the remaining mass of the sample are recorded. Three variations are commonly employed:

• Dynamic TGA – Temperature continues to increase over time as mass is recorded. This allows simulataneous identification of how much gas is removed and the temperature at which it occurs.
• Static TGA – Temperature is held constant as the mass is measured. This can be used to gain more information on a decomposition that happens at a certain temperature or to investigate a material’s ability to withstand a given temperature.
• Quasistatic TGA – Sample is heated in multiple temperature intervals, and held at those intervals for a time, often until the mass stabilizes. This is ideal for investigating substances that are known to decompose in various ways at different temperatures, and better characterizing the way in which they decompose.

How to interpret the data

Figure 1 shows a TGA curve in green. Figure from Physical Methods in Chemistry and Nanoscience by Pavan M.V. Raja and Andrew R. Barron (chemlibretext link).

Data from thermogravimetric analysis is often shown by a graph representing mass as a function of temperature for dynamic TGA. For static TGA, mass is instead plotted as a function of time at a given temperature. Quasistatic TGA produces multiple mass vs. time plots for various temperatures. The derivative of the mass change with temperature is often plotted on the same graph to improve ease of identifying the points at which different mass changes occur; especially helpful in cases where multiple decomposition reactions happen in close proximity to one another.

Examples of some characteristic TGA curves for dynamic TGA

Figure 1. Classification of the different observable TGA Curves. Image source

In general, mass fluctuations correspond to chemical reactions, with some exceptions. A common example is drying, which can easily be seen as a quick initial drop at the beginning of heating that isn’t known to correspond to any chemical reactions. Evaporation/sublimation may also appear on the plot depending on the material to be analyzed. Multistage decomposition is also common, and shows as a step-like pattern. In some cases, these steps may blend together during dynamic TGA, necessitating either far slower heating rates, or step-wise methods like quasistatic TGA. Note that TGA itself may not be sufficient to identify the decomposition products; chemical testing of the sample after TGA analysis is often required to ascertain the identities of suspected decomposition products. TGA itself does not identify substances; other methods such as chemical testing or differential calorimetry must performed alongside TGA to verify the identity of products. 

Good literature examples 

TGA is vital when designing materials that are intended to withstand high temperatures, as if there is even slight decomposition of the material at a temperature that the material would be expected to encounter, devices made of the material may fail over repeated use. The carefully controlled environment of the TGA analyzer also allows for measuring decomposition reaction kinetics. Differential scanning calorimetry can be incorporated into the TGA analyzer to allow for monitoring potential phase changes. Phase changes generally require addition of heat, yet do not increase the temperature of the sample undergoing a phase change. Furthermore, different phases of a material have different heat capacity, and the temperature change per joule of heat applied will vary with phase. By adding a reference pan to the TGA analyzer, changes in the heat capacity in addition to mass changes can be monitored. In this way, both phase changes and thermal decomposition reactions can be simultaneously measured by TGA.

TGA used for decomposition reaction:

Figure S6. Thermogravimetric analysis (TGA) under pure nitrogen flow at 100 mL/min to show a) clean decomposition of 3DP-HKUST-1gel and b) decomposition of 3DP-HKUST-1gelTEA showing that it has several side products during decomposition. (Lim et al. 2019)

Figure 2b. Thermogravimetric analysis (TGA) under simulated ambient conditions (SI section 5), showing desolvation followed by oxidation of 3DP-HKUST-1gel to CuO.

The authors are looking to use colloidal gels containing only ethanol and Cu3(BTC)2 (BTC = 1,3,5-benzenetricarboxylate) (HKUST-1) nanoparticles as ink for the direct ink writing (DIW) of pure densely packed and self-standing Metal-organic frameworks (MOF) monoliths. Traditionally they are synthesized in powder form. The authors are observing the decomposition behavior of the 3DP-HKUST-1gel (made using DIW) and 3DP-HKUST-1gel-TEA (made by triethylamine-induced HKUST-1 gels). It can be observed in the sudden change in weight over the 100-200 °C for Figure S6b that several side products have formed as oppsed to Figure S6a which shows a much cleaner decomposition. The Figure seen in the paper was Figure 2b, the authors attibute the first weight change (16.2 mg) to residual molecules such as H2O, acetate from the copper (II) acetate monohydrate precursor, and excess ethanolic solvent that is trapped inside the 3DP-HKUST-1gel structure. The second weight change (6.2 mg) was observed at 300 °C and is caused by the decomposition of the organic linkers and network. 

In-depth reading and works cited

1. Physical Methods in Chemistry and Nanoscience by Pavan M.V. Raja and Andrew R. Barron (chemlibretext link).
2. A Beginners Guide Thermogravimetric Analysis (TGA): A Beginners Guide to TGA that has FAQ and basic information.
3. Thermogravimetry Analysis (TGA) – online training course: Youtube training course that as good explanation about how the TGA works. Also has good examples of plots and how to understand them.
4. Thermogravimetric Analysis (TGA) & Differential Scanning Calorimetry (DSC): Slideshow with information about the TGA. Includes figures on classification of curves, how balance works, analyis of curves, effects of heat rate, shifts caused by heat rate, etc.
5. THERMAL ANALYSIS OF POLYMERS – Fundamentals and Applications: (WARNING!: This link will download a whole 388 pg. book!) Has a whole chapter dedicated to TGA.

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Vibrating Sample Magnetometry (VSM) is a measurement technique which allows to
determine the magnetic moment of a sample with very high precision. The aim of this
lab course M106 is to enlarge upon the use of this widespread technique introduced in
the lab course B512, where different ferromagnetic samples were characterized
concerning magnetic hysteresis and demagnetization. Here, we will gain a deeper
understanding of the behavior of magnetic materials and its measurement.

In order to
lay the foundations, first the measurement principle and the properties of ferromagnetic
materials will be summarized (magnetic domains, magnetic hysteresis,
demagnetization) and then we will elaborate on the magnetic anisotropy of
ferromagnetic materials.

A vibrating sample magnetometer (VSM) systems are used to measure the magnetic properties of materials. The vibrating component causes a change in the magnetic field of the sample, which generates an electrical field in a coil based on Faraday’s Law of Induction.

If the sample is placed within a uniform magnetic field H, a magnetization M will be induced in the sample. In a VSM, the sample is placed within suitably placed sensing coils, also held at the desired angle.

And the vibrating sample component is made to undergo sinusoidal motion, i.e., mechanically vibrated.

The hysteresis loop shows the “history dependent” nature of magnetization of a ferromagnetic material. Once the material has been driven to saturation, the magnetizing field can then be dropped to zero and the material will retain most of its magnetization (it remembers its history).

Procedure
Before using the VSM, you must carry out a series of configuration steps.
• Insert the Ni standard into the VSM. The standard is ball-shaped, therefore
magnetically isotropic, and has a magnetic moment of 6.92 emu at 5000 Oe.
• Find the exact position of the standard in respect to the center of the pickup coils. The
vibrating rod can be adjusted by three screws on top of the VSM for x, y and z
direction. The pickup coils are connected in a way that, the sample being in the center
of the coils, there will be a signal minimum along x-, a maximum along y- and a
maximum again along z-direction.
• Run Calibrations → Moment gain to calibrate the instrument, i.e. to convert the
measured voltage signal into the correct value of the magnetic moment.
After calibration of the VSM, the following measurements aim to address two topics. The
first part covers basic magnetic characterization and the information that can be
deduced from magnetization curves. The second part cope with demagnetization.

1. Magnetocrystaline anisotropy energy:
   Fix the Fe single crystal to the sample holder. Set H0 to 3500 G and record the
   magnetic moment of the crystal during a 360° rotation of the sample.
   Find the angles corresponding to the different crystallographhic / magnetic axes and
   record the magnetization curves of the easy axis and the hard axis.
2. Stress induced magnetic anisotropy
   Mount a sheet sample clamped in a sample holder provided by the supervisor into the
   VSM. Record the magnetization curves of the sample with and without applied stress
   along and perpendicular to the stress direction.
   Determine the volume of each sample that you have measured

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Operation

A sample is made to oscillate using a vibrational unit extended on a rod. The sample is placed between two electromagnetic pieces which are used as the applied field for this this experiment. With the sample oscillating induces a voltage between the search coils which creates a signal to determine the magnetic properties of the sample. Reference coils are used to create a reference signal such that noise generated from the signal can be filtered using a lock-in amplifier [1]. Because the signal and the reference signal are directly related through its voltage and amplitude means that precise measurements can be recorded using a voltmeter. Calibration methods are important to determine the relation between the voltages induced by the magnetic field and the sample and their magnetic properties.

Calibrating the applied field is done by increasing the voltage in steps measuring the field until reaching a maximum. The system is calibrated using a nickel standard normally as a number of volts per unit of magnetic moment. Many materials such as types of barium ferrite or alnico materials can be placed inside to determine properties. These properties include remanence, coercivity, intrinsic coercivity and operating points once the system has been calibrated.

Advantages and Disadvantages in terms of experimental facets

The key advantage is the precision and accuracy of VSMs. Taking measurements at a range of angles once detection arrangements for the coils have been devised can be done. The advantage of sample vibration perpendicularly to the applied field can be found once the detection coils have been arranged appropriately. This means that there is the ability to test the sample at different angles. The positioning of the coils are done in a way to reduce the effects of sample position variation and external field variation- essentially deep into the applied field shown in figure 1. Disadvantages are that they are not well suited for determining the magnetisation loop or the hysteresis curve due to the demagnetising effects of the sample. Another problem is that, particularly for the VSM used in the third year laboratory is that temperature dependence cannot be controlled.

Figure 1. A schematic layout of the VSM

2. B-H Hysteresis Loop Tracer

Operation

The B-H hysteresis loop tracer is essentially two coils, one with a sample and the other which is empty for comparison. The insertion of a sample into the pickup coils causes a voltage proportional to the rate of change of the vector field to occur across the difference amplifier. After passing through an integrator, a voltage proportional to the intrinsic induction is passed to the Y-amp of the oscilloscope. This voltage combined with an X-voltage representing the magnetising field generated from the solenoid without the sample results in the generation of a hysteresis loop on the oscilloscope. Calibration is through a balance and phase adjustment to establish a trace on the oscilloscope. They are done to make sure that the magnetising field is linear and that every vector corresponds to the applied field. Measurements for the magnetic properties can then be made.

Advantages and disadvantages in terms of experimental facets

The coils have the ability to heat the sample such that temperature variance can be observed in the way that the material behaves when influenced by a magnetic field. On the other hand, this could cause overheating of the system which could result in a failure. Using a BH-looper can give the user a more improved visualisation compared to a VSM of the way a material behaves. The values plotted on the scope are only proportional to the absolute values, therefore display yields qualitative not quantitative information about a material magnetic properties. The precision is generally low compared to a VSM. Because a hysteresis loop is viewed using an oscilloscope means that observations of whether the material is a soft or hard magnetic material. And this is why it is used in quality control testing industries like the control of ferromagnetic oxides in a magnetic tape factory.

Figure 2. A schematic layout of a BH loop tracer [2].

3(I) Difference between concepts of Vector Field B, Magnetisation M and the magnetising field H

The vector field B represents the magnetic induction. Magnetisation M is the magnetic moment per unit volume of a solid. Magnetising H field is the magnetic field strength. These three quantities are related by the equation.

With μ₀ being the permittivity of free space. To show the difference between these quantities, hysteresis loops for a magnetic material shown in figure 4 are used. One of the key differences shown is that the magnetisation saturates whereas the B field increases at a constant rate for certain values for H. The magnetisation is generated by the spin and the orbital angular momentum of electrons in the solid. H is generated outside the material by electrical currents[3]. Therefore, from the equation above, the B field is the combination of H and M which shows the difference between the quantities with the inclusion of the permittivity of free space.Find out how UKEssays.com can help you!

A way to show the difference between the 3 parameters is through the representation of a bar magnet in a magnetic field shown in figure 3. Unfortunately, due to the age of the diagram, the labels are a bit old. Hence the ‘True’ field denotes the vector field B and the Applied field represents the magnetisation M. However, the arrows represent the direction and strength of each parameter. It is clear from figure 3 that the Magnetisation is much stronger than the demagnetising field.

Figure 3 An example of a magnet being demagnetised in an applied field

From figure 4, the two sketches representing of B and M against H can give an understanding of other magnetic properties of the material. The curve on the left can show the saturation of the magnetic material as well as the remanence M_r– the remaining magnetisation after the applied field has been turned off. The right hand diagram can show the remanent induction B_r and the saturation point of the applied field. In terms of the difference between the parameters, M, B and H, they yield different properties of the material in question.

Figure 4 Hysteresis loops showing (a) M and (b) B field against H

3(II) The difference between the susceptibility and relative permeability

The relative permeability μ_r and susceptibility χ are very closely related as shown by the equation below:

The relative permeability represents a characterisation of magnetic materials. Paramagnetic or diamagnetic materials have permeabilities close to the permeability of free space. However for ferromagnetic materials, the permeability is large in comparison. It represents a multiplication factor. For example, the use of an iron core with a relative permeability is 200 times greater than just an air coil used. So this is a measure of the actual magnetic field within a ferromagnetic material. Susceptibility is a measure to an extent to which a material may be magnetised in a magnetic field. It represents a ratio of how much a material is magnetised compared to the applied field on that material [4]. So the susceptibility specifies how much the relative permeability differs from one as shown in the equation above.

References

[1] Foner S 1959 Versatile and Sensitive Vibrating-Sample Magnetometer* Rev. Sci. Instrum. 30 548–57

[2] Howling D H 1956 Simple 60-cps Hysteresis Loop Tracer for Magnetic Materials of High or Low Permeability Rev. Sci. Instrum. 27 952

[3] Jiles D 1990 Introduction to Magnetism and Magnetic Materials (Chapman and Hall)

[4] Magnetic Susceptibilty http://www.britannica.com/EBchecked/topic/357313/magnetic-susceptibility

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Increasing media storage density continues to be a very active area of research. Magnetic media may be divided into particulate and continuous media.

Particulate media are comprised of small magnetic particles bonded on a plastic tape or disk, the thickness of the magnetic overcoat is typically on the order of 10,000 Å. Since these are single domain particles, the information is stored by inverting the magnetization of some of the particles. Continuous media are metallic thin films, typically a few hundred angstroms in thickness. Particulate media are advantageous in that they are relatively simple to prepare and are chemically stable, however their recording density is relatively low.

Continuous media on the other hand have higher storage densities and the shapes of their hysteresis loops (and hence recording characteristics) may be varied in a controlled way.

Hard and Soft Magnetic Materials

Magnetic materials are classified into two broad categories, soft or hard. Soft magnetic materials are characterized by large permeabilities and very small coercivities, typically less than 1 Oe. Hard magnetic materials are most often used in permanent magnet applications, and are characterized by large saturation magnetizations, large coercivities, typically greater than 10 kOe, and also by large energy products (i.e., BHmax). Intermediate magnetic materials are generally characterized by coercivities on the order of 1 kOe, and these materials are usually used in magnetic media.

Intermediate magnetic materials include; Gamma-Fe₂O₃, Co₈₀Cr₂₀, Co₇₇Ni₁₀O₁₃, and thin films. The characteristics of any magnetic material, whether it is hard, soft, or intermediate, are best described in terms of their hysteresis loop. The most common measurement method employed for hysteresis loop determinations at ambient temperature is the Vibrating Sample Magnetometer (VSM).

This paper will discuss the utility of the VSM in the characterization of magnetic media materials. We will limit our discussion to longitudinal recording media, i.e., where the magnetization is parallel to the plane defined by the substrate/film. Perpendicular media, where the magnetization is perpendicular to the plane defined by the substrate/film, and magneto-optical materials are currently enjoying considerable research effort because of their potential for increasing areal storage densities.

Vibrating Sample Magnetometer (VSM) Systems

Vibrating Sample Magnetometer (VSM) systems are used to measure the magnetic properties of materials as a function of magnetic field, temperature, and time. They are ideally suited for research and development, production testing, quality and process control. Powders, solids, liquids, single crystals, and thin films are all readily accommodated in a VSM.

Contemporary commercial VSM’s feature virtually automated operation via data acquisition/control and analysis software that runs on a personal computer, thus making the VSM accessible to the non-specialist. This has dramatically increased the utility of this measurement technique in a broad range of measurement applications.

Theory of Operation of Vibrating Sample Magnetometer Systems

If a material is placed within a uniform magnetic field H, a magnetic moment m will be induced in the sample. In a VSM, a sample is placed within suitably placed sensing coils, and is made to undergo sinusoidal motion, i.e., mechanically vibrated. The resulting magnetic flux changes induce a voltage in the sensing coils that is proportional to the magnetic moment of the sample.

The magnetic field may be generated by an electromagnet, or a superconducting magnet. Variable temperatures may be achieved using either cryostats or furnace assemblies. In the context of the current discussion, we will consider electromagnet based systems only, as magnetic media are usually characterized at ambient temperature, and for only moderate field strengths. Tape and thin film samples to 1 inch in diameter may be characterized in the Lake Shore VSM.

The Hysteresis Loop

In the case of a typical recording medium the hysteresis loop gives the relation between the magnetization M and the applied field H. A hysteresis loop of a magnetic recording medium is illustrated schematically in Figure 1.

The parameters extracted from the hysteresis loop that are most often used to characterize the magnetic properties of magnetic media include; the saturation magnetization Ms, the remanence Mr, the coercivity Hc, the squareness ratio SQR, S* which is related to the slope at Hc , and the switching field distribution SFD. The loop illustrated in Figure 1 shows the behavior for the easy axis of magnetization (i.e., in the anisotropy direction). The loop has a rectangular shape and exhibits irreversible changes of the magnetization.

The hard axis loop, where the hard axis is at right angles to the easy axis, is more or less linear and generally hysteresis free, i.e., the magnetization is reversible. Magnetic materials that show a preferential direction for the alignment of magnetization are said to be magnetically anisotropic. When a material has a single easy and hard axis, the material is said to be uniaxially anisotropic.

The intrinsic saturation is approached at high H, and at zero-field the remanence is reached. The squareness ratio is given by the ratio of (M_r/M_s) and is essentially a measure of how square the hysteresis loop is.

In general, large SQR values are desired for recording medium. The formal definition of the coercivity Hc is the field required to reduce the magnetization to zero after saturation. The physical meaning of Hc is dependent on the magnetization process, and may be the nucleation field, domain wall coercive field, or anisotropy field.

H_c is a very complicated parameter for magnetic films and is related to the reversal mechanism and the magnetic microstructure, i.e., shape and dimensions of the crystallites, nature of the boundaries, and also the surface and initial layer properties, etc.

Parameters of Importance to Magnetic Media

S* and SFD are of particular importance in characterizing the magnetic properties of magnetic media. S* is related to the slope of the hysteresis loop at Hc, i.e., dM/dH|H_c = M_r/(H_c(1 – S*)). This is known as the Williams-Comstock construction. For longitudinal recording media there are two important parameters associated with the recording process that are intimately related to S*.

Namely, the maximum output signal depends on Mr, Hc, and S*, and the optimal bias current also depends on S*. The SFD = ΔH/Hc where ΔH is the full width at half maximum of the differentiated curve dM/dH (as illustrated in Figure 1) can be thought of as a distribution function of the number of units reversing at a certain field. For a particulate medium without collective behavior, the SFD has a close relation to particle size distribution because differently sized and shaped particles will reverse at different field strengths.

For longitudinal media the SFD is related to recording parameters such as noise, optimal bias current, and time dependent behavior. Media with high Hc and small SFD are desirable for high density recording.

Remanence Curves

In addition to the full hysteresis loop properties of magnetic media, there has been increased interest in the measurement of remanence curves. Measurement of remanence determines only the irreversible component of magnetization and thus enables the phenomena of switching to be deconvoluted from the hysteresis measurement, which generally includes a reversible component.

There are two principle remanence curves; the isothermal remanence (IRM) and the DC demagnetization curve (DCD). The IRM is measured after the application and removal of a field with the sample initially demagnetized. The DCD is measured from the saturated state by application of increasing demagnetizing fields. Both are illustrated schematically in Figure 2. These remanence curves are of importance because they yield the true SFD for the material. The VSM may also be used to measure the IRM and DCD remanence curves.

The remainder of this paper will present magnetic data for thin film magnetic media, thus demonstrating the utility of the Lake Shore VSM for measuring media magnetic properties.

Magnetic Measurements Using the Lake Shore VSM

The Lake Shore VSM features variable-gap electromagnets providing field strengths to over 2 tesla. Experimental flexibility, both in terms of achievable field strengths, and in terms of allowable sample sizes are provided since the gap spacing may be adjusted to maximize either.

Auto-rotation and Vector options facilitate investigations of anisotropy in magnetic media. With the auto-rotation option the sample may be rotated such that the applied field is oriented parallel to either the easy or hard axis of magnetization, or at any angle in between. The Vector option, which includes 2-axis or 3-axis coil sets placed at right angles to one another, permits simultaneous measurement of both easy and hard axis magnetization for fields oriented parallel to either axis. This option also permits the derivation of torque since torque is equal to the cross product of the field and magnetization vectors (i.e., t = M x H).

Data collection is fully automated with Windows based data acquisition/control and analysis software. Broad application versatility is maintained since measurement parameters may be easily defined and controlled. The software automatically extracts any of a number of parameters, e.g., Ms, Mr, Hc, SQR, S*, SFD, etc., directly from the measured hysteresis loop. And, extensive data analysis capabilities are also provided, e.g., derivative (SFD) curves, substrate and paramagnetic background corrections, etc.

Measurement Results

Hysteresis Loops for a Thick Film Disk Material

Figure 3 shows the initial, minor, and major hysteresis loop for a thin film disk material. In the context of the present discussion, the minor loops of magnetic media are sometimes of interest as they relate to modeling of the write process. Taken together with the major loop, the minimum head field strength required to ensure saturation and hence maximum remanence are determined.

Magnetization Curve, Major Hysteresis Loop and Remanence Curve for a Flexible Magnetic Media Material

Figure 4 shows the initial magnetization curve, major hysteresis loop, and also the DCD demagnetization or remanence curve for a flexible magnetic media material.

Major Hysteresis Loop for a Flexible Media Material

Figure 5 shows the major hysteresis loop for a flexible media material, and the derivative curves are also illustrated. These derivative curves are directly related to S* and the SFD. Since small SFD’s are desirable, the sharpness and width of these derivative curves are of interest. A narrow and stable switching transition produces a small SFD, and hence the derivative curves yield useful information concerning the magnetic structure of the media, which in turn is related to the microstructure and chemical inhomogeneities in the layer. These parameters are principally related to the deposition process itself.

Isothermal Remanence (IRM) and DC Demagnetization (DCD) Remanence Curves for a Flexible Media Material

Figure 6 shows the isothermal remanence (IRM) and DC demagnetization (DCD) remanence curves for a flexible media material. Interaction effects may be investigated by analyzing these curves. If the particulate media is characterized by non-interacting particles then a Henkel plot, i.e. IRM(H) vs. DCD(H), will be linear, and the forward and reverse SFD’s will be identical. Deviations from linearity are attributable to the effects of interactions in the system.

Figure 7 shows the Henkel plot corresponding to Figure 6 and Figure 8 illustrates the forward and reverse SFD’s obtained from differentiation of the IRM and DCD curves. Clearly the SFDs are not identical. The extent to which interactions exist in the system are revealed by these types of ΔM vs H curves. A larger interaction yields a larger ΔM peak. The use of this type of analysis is becoming increasingly common in the investigation of interaction effects in particulate and thin film media. A strong correlation exists between the form of these interaction effects, and the degree of dispersion of the particles.

Hysteresis Loop for Hard Disk Magnetic Film

Figure 9 shows a hysteresis loop for hard disk CoPt magnetic film deposited on a rigid disk substrate. Critical M(H) loop parameters are indicated in the figure.

Figures 10 and 11 show the hysteresis loop and derivative curve, respectively, for a hard disk film sample.

Summary

Selecting a VSM and Future Requirements

There are a number of considerations that come into play when selecting an appropriate VSM. These include; the types of materials that are to be measured, i.e., both intrinsic magnetic characteristics and physical properties and dimensions are important, required magnetic field strength, accessible temperature range, available measurement options, ease-of- use which is largely dictated by the software interface, etc.

Current research trends in magnetic media include the development of perpendicular recording media, magneto-optical materials, the development of pseudo-contact recording techniques, the use of magnetoresistive (i.e., GMR and CMR) multi-layer films for read heads, the use of alternative substrate materials (e.g., glass), and patterned media. Additionally, the superparamagnetic limit is being approached as magnetic film thicknesses are decreased. This trend will force VSM manufacturers to enhance the sensitivity characteristics of their VSM’s.

This paper has discussed some of the more important magnetic properties of magnetic media, their relation to the recording process, and their determination utilizing a Vibrating Sample Magnetometer measurement methodology. The wide spread use of magnetic media materials for audio, video, and data storage systems results in a continual research effort to increase storage densities, and decrease access time.

Advances made possible by materials science, combined with the development of commercially available computer automated characterization tools, such as the VSM will certainly result in significant advances in this area.

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TGA is a powerful and robust technique to explore the thermal stability of a material. By accurately monitoring the weight of a sample while heating at a constant rate, we can measure changes in a sample’s weight and attribute this to a specific material response to a thermal stress (Figure 1). This is perfect for exploring, in detail, decomposition temperatures and ensuring a material performs adequately in a given temperature range.

During a test, a carrier gas flows over the sample and the weighing mechanism.  This carrier gas serves two purposes: protecting the internals from corrosion/oxidation above 500 °C, and to interact with the sample through gas-solid or gas-liquid reactions. By providing an inert atmosphere, we can test the thermal stability of a material. Reducing environments can explore gas-solid phase reduction reactions or protect specific samples from being oxidized. By the nature of the sensitivity of the TGA balance, we also can observe the absorption of gas onto a porous material at various temperatures. This is an ideal technique for exploring metal organic frameworks, or catalytic porous materials. Owing to the sensitivity of the balance on our SETARAM Labsys Evo instrument, we have ideal sensitivity for running thermokinetic experiments. This experiment has applications towards thermal stability of a given material at elevated temperatures.

The SETARAM Labsys offers the ability to perform TGA analysis up to 1600 °C and additionally under a variety of gas mixtures due to our gas-mixing option.

Differential Scanning Calorimetry (DSC)

DSC is a flexible technique to explore thermal transitions within a given sample. By heating a sample and measuring the heat flow as compared to a reference standard, we can access thermoanalytical information on a given material. DSC curves are generated by plotting heat flow (mW) vs sample temperature (°C), and an example plot is found in Figure 2, and demonstrates the melting and fusion of Indium Corp. Indalloy 80Au/20Sn solder. In this case, we observe a phase change (solid-liquid followed by liquid-solid); however, we can also observe other thermal transitions within a material, such as evaporation, thermal transitions between polymorphs, and determination of key thermal constants. One of these key thermal constants is heat capacity (Cp), which an be difficult to acquire due to the demanding experiment required to gain access to this information. Heat capacity requires precise and very specific sensitivity of the DSC sensor, as it is a very small and difficult thermal effect to capture effectively. Owing to our 3D Calvet type sensor on our µDSC 7, we have the capability to measure such small thermal effects (0.02 µW) requiring the upmost sensitivity and precision from 0 – 120 °C. For higher temperatures, our SETARAM Labsys Evo instrument has a specifically designed 3D-psuedo-Calvet sensor, which allows TAL to perform C_p testing with better than 2% accuracy from ambient temperatures to 1600 °C. This very sensitive and difficult to determine thermal effects also include the glass transition point (T_g), water state in materials and other thermodynamic and thermokinetic effects.

Differential Thermal Analysis (DTA)

DTA is a similar technique to DSC, however instead of measuring the heat flow between the furnace temperature and the sample, you measure the temperature difference between a sample and a standard reference using thermocouples. This is particularly useful for phase-change materials and the study of organic and polymeric materials using analytical precision. Owing to the more sensitive detector within typical DTA sensors, DTA testing is particularly useful for running thermokinetic experiments due to the lower thermal inertial barrier. TAL offers DTA testing from ambient to 1200 °C, allowing us to explore thermal effects at elevated temperature, capabilities which we have newly acquired.

While each of these techniques may be used to probe into a single physical characteristic of a material, the real power we provide is simultaneous thermal analysis techniques for niche applications on a single sample. With TAL’s Labsys Evo 1600 and DSC 131, we offer capabilities to include high temperature ranges with mixtures of gases. For example, TAL offers TGA, DSC and DTA experiments from ambient temperatures up to 1600 °C. Figure 3 shows a TGA-DSC decomposition experiment captured on our Setaram Labsys Evo apparatus, where CuSO₄•5H₂O decomposition can be measured by TGA (water, SO₂ and O₂) and DSC. In addition to these coupled thermal experiments, we offer the capacity to provide gas mixtures for high precision control over the exact atmospheric exposure during thermal analysis runs. TAL also offers the capacity to run samples under vacuum (10^-3 Bar) using our Labsys Evo system, which is useful for isolating gas-sample interactions. TAL also offers pressurized DSC experimentation, allowing for the study of various samples under 200 psi. This can provide insight into thermal transitions under pressure, such as those in the oil and fuel industry or in the case of high-pressure lubricants.