Differential Scanning Calorimetry Peak Research Articles

Two-Step Synthesis of VO2 (M) with Tuned Crystallinity

Highly crystallized monoclinic vanadium dioxide, VO2 (M), is successfully synthesized by a two-step thermal treatment: thermolysis of vanadyl ethylene glycolate (VEG) and postannealing of the poorly crystallized VO2 powder. In the first thermolysis step, the decomposition of VEG at 300 °C is investigated by X-ray diffraction and scanning electron microscopy (SEM). A poorly crystallized VO2 powder is obtained at a strict time of 3 min, and it is found that the residual carbon content in the powder played a critical role in the post crystallization of VO2 (M). After postannealing at 500 and 700 °C in an oxygen-free atmosphere, VO2 particles of various morphologies, of which the crystallite size increases with increasing temperature, are observed by SEM and transmission electron microscopy. The weight percent of crystalline VO2, calculated using the Fullprof program, increases from 44% to 79% and 100% after postannealing. The improved crystallinity leads to an improvement in metal-insulator transition behaviors demonstrated by sharper and more intense differential scanning calorimetry peaks. Moreover, V2O3 and V2O5 with novel and particular microstructures are also successfully prepared with a similar two-step method using postannealing treatment under reductive or oxidizing atmospheres, respectively.

Simple Strategy for Dual Control of Crystallization and Thermal Property on Polyesters by Dispersing Metal Salts Via Multiple Coordination Bonds

AbstractIn this study, metallo‐supramolecular polyesters with multiple coordination bonds along the chains are prepared, to demonstrate a simple strategy to control both the thermal property and crystallizability. Firstly, polyesters with multiple pyridine‐ligands are synthesized through melt polycondensation and subsequent Michael addition reaction. By adding a metal salt (ZnCl2), the fraction of metal‐coordinated pyridine‐ligands is systematically increased with increasing the Zn2+/pyridine‐ligands mole ratio according to Fourier transform infrared spectroscopy (FT‐IR) measurements, which is found to play a role in tuning the glass transition temperature. The metal‐ligand coordination simultaneously causes the disappearance of crystallization/melting peaks in differential scanning calorimetry (DSC) thermograms, and scattering measurements also indicate the disappearance of crystalline domains. A transparent film is thus obtained after blending small amounts of ZnCl2 (≪10 wt%), although the neat crystalline sample is highly opaque. This non‐crystallization phenomenon is induced by inhibition of the chain arrangement due to the existence of metal salts dispersed via coordination with pyridine‐ligands. By changing the fraction of pyridine‐ligands in the chain, it is found that the wider temperature range Tg tuning can be achieved for samples with higher ligand fractions.

Synthesis and characterization of benzocyclobutene-terminated imides with high organosolubility

Benzocyclobutene resins play an important role in microelectronic industry owing to their excellent physical and chemical properties. In our work, three novel benzocyclobutene-terminated imide monomers were synthesized via the reaction of 1-aminomethyl benzocyclobutene with various aromatic dianhydrides. The monomers exhibited good processability with superior solubility and low melting points (<163.5 °C), and they showed similar curing behaviors under N2 with an exothermic peak in differential scanning calorimetry (DSC) curves ranging from 217.3 °C to 287.7 °C. Highly crosslinked resins obtained at 150–300 °C exhibited superior tensile strength (>74.3 MPa), outstanding thermal stability (Td > 466 °C in N2), high glass transition temperature (>278 °C), high storage modulus (>3.25 GPa at 30 °C), low dielectric constant (<3.07 at 1 MHz) and good water resistance (the water absorption was below 0.81% after immersed in water for 24 h and the water contact angle was higher than 86.6°). Atomic force microscopy demonstrated the perfect uniformity and planarity of the cured films.

A feasible method to measure the content of core and shell in heterostructural perovskite MOFs through differential scanning calorimetry

The core-shell heterostructures of [(CH3)2NH2][Mn(HCOO)3]@ [(CH3)2NH2][Co(HCOO)3] and [(CH3)2NH2][Mn(HCOO)3]@[(CH3)2NH2][Ni(HCOO)3] were prepared via epitaxial growth. The obtained heterostructural crystals were characterized by single-crystal and powder X-ray diffraction analysis, and energy dispersive spectrometer (EDS) elemental mappings. Investigation on the differential scanning calorimetry (DSC) of the heterostructural crystals with different mole ratio of the core to shell indicates that the plot of DSC peak area versus mole ratio of core to shell exhibits a linear relationship. Thus, to an unknown heterostructural compounds with distinct phase transition, the mole ratio of core to shell can be easily obtained just by measuring their DSC data.

Determination of the Crystallization Behavior of Lipids by Temperature Modulated Optical Refractometry

This study was conducted to examine if the new temperature modulated optical refractometry (TMOR) method is applicable to study the phase behavior of alkyl-based components. n-Hexadecane, palmitic acid, and glycerol tripalmitate were used as model components. TMOR was benchmarked against differential scanning calorimetry (DSC) and polarized light microscopy (PLM). For all substances, a good agreement of the DSC data with TMOR was found. For n-hexadecane, a difference of 2.2 °C for the crystallization and 2.6 °C for the melting temperature was found. Considering palmitic acid, the crystallization temperature differed by 3.3 °C while the melting varied by 2.8 °C. The crystallization temperature of tripalmitate identified by TMOR was 2.7 °C higher, and the melting temperature 2.3 °C was lower compared to the DSC. The crystallization temperature for TMOR was always higher, and the melting temperature was always lower if related to DSC. This leads to the conclusion that TMOR is more accurate and direct. In addition, the transition peaks identified by TMOR were narrower compared to the DSC peaks. This is due to slower heating and cooling rates leading to a smaller temperature range of phase transition and less thermal lag. The study showed that TMOR is an appropriate method to determine the phase transition temperatures for the three examined substances. The results were comparable to the DSC data in both melting and crystallization behavior. Since the accuracy of TMOR is better at lower heating and cooling rates, it could be a reasonable extension of the well-known DSC method in the studies of melting and crystallization.

Glass stability (GS) of chemically complex (natural) sub-alkaline glasses

Glass stability (GS) indicates the glass reluctance or ability to crystallise upon heating and it can be characterised by several methods and parameters. GS is frequently used to retrieve glass-forming ability (GFA) of corresponding liquids: the likelihood of obtaining a crystal-free glass through melt-quenching.In the present study, GS has been determined for the first time on six sub-alkaline glasses having complex (natural) compositions, the most widespread and abundant on Earth. The two end-members are a basalt and a rhyolite, B100 and R100, plus intermediate compounds B80R20, B60R40, B40R60, B20R80. Each glass was heated in a differential scanning calorimetry (DSC) at a rate of 10°C/min (600°C/h) to measure in-situ Tg (glass transition), Tx (onset of crystallization) and Tm (melting) temperatures, from ambient to their liquidus temperatures. The ex-situ run-products quenched at Tm have been characterised by scanning electron microscope (SEM) and electron probe micro-analyzer (EPMA) techniques, in order to quantify textures and compositions of phases, respectively.R100 and B20R80 do not shown any DSC peaks, whereas B40R60, B60R40, B80R20 and B100 thermograms display progressively more resolvable peaks. As SiO2 (wt%) in the melt increases from B100 to B40R60, Tx linearly increases, Tm first decreases and then levels off, whereas Tg weakly changes. R100 and B20R80 run-products are completely glassy, while from B100 to B40R60 the amount of glass (gl) increases from 48.5 to 97 area%, counterbalanced by a decrease of clinopyroxene (cpx) content from 47.7 to 16 area%. The spinel (sp) content is constrained within a narrow range of 0.9–3.8 area%. Conversely, plagioclase (plg) crystallizes heterogeneously on the Al2O3 holders only in B100 and B80R20 and at distance <100μm from it. R100, B20R80, B40R60 and B60R40ex-situ glasses exhibit chemistries very close to their starting compositions, according to the absence (or scarcity) of crystals formed during heating. Instead, B100 and B80R20 glasses are enriched in Si, Al, and Na but depleted in Fe, Mg, and Ca due to internal crystallization of sp and mostly cpx. Specifically, the composition of cpx from B100 is enriched in M2Ca, M1Mg, M2,M1Fe, and M1,TAl.The values of KT, KH, KW, KLL, and w2 (as GS parameters) increase linearly and monotonically as a function of SiO2, showing high correlation coefficients (R2=0.93–0.95). Moreover, Tx values and GS parameters highly correlate with GFA via Rc (critical cooling rate), as previously determined by ex-situ cooling-induced experiments. This leads to the conclusion that GS scales with GFA for natural silicate compositions. In addition, the in-situ Rc value of B100 measured with DSC is >45°C/min (>2700°C/h), corroborating the value of Rc of ~150°C/min (9000°C/h) determined by ex-situ experiments. In turn, relevant solidification parameters on heating or cooling obtained by DSC investigations, also for chemically complex (natural) systems, extend the results from previous observations conducted on simple silicate systems. These outcomes are relevant for lavas or magmas that re-heat glass-bearing volcanic rocks, as well as for fabricating glass-ceramic materials with desirable texture and composition of phases starting from abundant and very cheap raw volcanic rocks.

Thermoanalytical Study of Linkage Isomerism in Coordination Compounds. Part 7. A DSC and DFT Investigation of Solid-state Linkage Isomerization in Bis(thiocyanato)-bipyridineplatinum(II) Complex

The linkage isomerization of [Pt(SCN)2(bipy)] complex in solid-state was investigated by differential scanning calorimetry (DSC) at diverse heating rates. The conversion of the bis-thiocyanato isomer (–SCN)2 to the bis-isothiocyanato isomer (–NCS)2 was accompanied by the appearance of an exothermic peak. However, no DSC peak was obtained for isomerization of the (–NCS)2. The results imply that the (–SCN)2 isomer is metastable which can convert to the stable isomer (–NCS)2 at elevated temperatures. Assuming a two-stage irreversible isomerization, the enthalpy changes of the first stage ΔHSCN1 and also second stage ΔHSCN2 isomerization were obtained (–2.99 ± 0.44 and –2.81 ± 0.45 kJ·mol–1, respectively) using the mathematical resolution of the observed DSC peaks. The thermokinetic parameters of this conversion were determined using Kissinger method. The activation energy values for the first and second stages of isomerization are evaluated, 101.78 ± 7.58 and 106.26 ± 5.87 kJ·mol–1, respectively. The low values of the activation enthalpy, ΔH‡ and the high negative activation entropy ΔS‡, obtained by Eyring equation, supported an associative mechanism. A DFT study was employed to detect the electronic structures and the thermodynamic stabilities of the three linkage isomers and the transition states.

Analysis of Compositional Modification of Commercial Aluminum Bronzes to Obtain Functional Shape Memory Properties

In copper-based shape memory alloys (SMAs), some exceptional phenomena, such as the shape memory effect (SME) or superelasticity (SE), are observable. However, commercial aluminum bronzes, Cu3Al-based alloys, do not present these functional properties (SME and/or SE) in their original state. Thus, since one of the main copper-based SMA systems is the Cu-Al-Ni alloy, this paper aims to analyze the modification of these commercial aluminum bronzes to SMA by the addition small amounts of Cu, Al and/or Ni. These modified bronzes were reprocessed by induction melting and injected by centrifugation into a ceramic coating mold. The modifications were made to determine the nominal composition for a Cu-13,0Al-4,0Ni (%wt) SMA. The effectiveness of the modifications was verified by differential scanning calorimetry (DSC) thermal analysis. All modified Cu-Al-Ni bronzes presented DSC peaks of the thermoelastic martensitic phase transformation, showing that SMA behavior was achieved, while the non-modified bronzes revealed no transformation. These results were supported by Vickers hardness (HV), X-ray diffraction (XRD), semi quantitative composition by EDS analysis and optical microscopy.

Stored energy in ultrafine-grained 316L stainless steel processed by high-pressure torsion

The energy stored in severely deformed ultrafine-grained (UFG) 316L stainless steel was investigated by differential scanning calorimetry (DSC). A sample was processed by high-pressure torsion (HPT) for N=10 turns. In the DSC thermogram, two peaks were observed. The first peak was exothermic and related to the annihilation of vacancies and dislocations. During this recovery, the phase composition and the average grain size were practically unchanged. The energy stored in dislocations was calculated and compared with the heat released in the exothermic DSC peak. The difference was related to the annihilation of vacancy-like defects with a concentration of ∼5.2×10−4. The second DSC peak was endothermic which was caused by a reversion of α′-martensite into γ-austenite, however in this temperature range dislocation annihilation and a moderate grain growth also occurred. The specific energy of the reverse martensitic phase transformation was determined as about −11.7J/g.

Proton-irradiation-induced structural and magnetic property changes in Ni–Mn–Ga high-temperature shape memory films

Ni51.90Mn28.86Ga19.24 alloy films were irradiated by 120keV protons at different fluences to investigate the effect of irradiation on their crystal structure, phase-transition temperature, and magnetic properties. The results show not only that a nanoscale amorphous layer may have been induced on the surface, but also that non-modulated (NM) martensite was produced. Moreover, differential scanning calorimetry peaks of the martensitic and austenitic transition temperatures are shifted to higher temperatures after irradiation; in particular, two endothermic and two exothermic peaks were observed for a proton fluence of 2.0×1016/cm2. Further, the formation of NM martensite could produce an extra shoulder on the M–T curves of the irradiated films. Regarding the magnetic properties, a gradual decrease in the Curie temperature TC can be caused by irradiation at a higher proton fluence. The changes in the saturation magnetization Ms with the proton fluence seem to be related to the reduction in TC.

DSC investigation of bovine hide collagen at varying degrees of crosslinking and humidities

Bovine hide collagen (nonCLC; non-CrossLinked Collagen) was analysed by differential scanning calorimetry (DSC) at different hydration degrees and compared with hide collagen samples crosslinked with glutaraldehyde (CLC-GA) and chromium(III) ions (CLC-Cr), respectively. Crosslinking and drying were confirmed to increase the denaturation temperature. Different regions were assigned, that reflect the variation of the influence of water on the denaturation temperature. Furthermore, at moderate hydration degrees, the enthalpies of non-crosslinked collagen increase compared to the fully hydrated state. This reflects a glue-like action of water in the range of 25% hydration. Crosslinking of bovine hide collagen decreases the enthalpy by 25% in the fully hydrated state, even at very low levels of crosslinking This can be explained by intensive effects of the crosslinking agent on the hydration network of the collagen molecules, assuming that the enthalpies are principally a result of hydrogen bonding. At very low water contents DSC peaks of CLC-Cr completely disappear. This could be explained by competition between hydroxosulfochromate(III) complexes and collagen for water.

Investigating aging effects for porous silicon energetic materials

When infused with an oxidizer, on-chip porous silicon (PS) shows tremendous potential as an energetic material. However, applications such as fuzing and propulsion require long-term material stability. The present work utilizes accelerated lifetime testing for PS samples with sodium perchlorate (NaClO4) oxidizer. Devices were exposed to elevated temperatures for various time intervals, then subjected to an electrical pulse through an integrated bridgewire to test for ignition. The pass/fail data from ignition testing was then analyzed to determine the mean and median failure point at each temperature using an Arrhenius aging model and a lognormal probability density function (PDF). Samples were heated over a temperature range of 185–300 °C for up to 46 h with median failure times ranging from 0.4–20 h. Differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR) spectroscopy were used to evaluate chemical changes of PS/NaClO4 during aging. Comparison of DSC traces for aged samples showed differences for heating above and below 250 °C, suggesting two different aging mechanisms. FTIR results suggest that for low temperature aging (below ∼250 °C) the hydrogen termination layer of the porous silicon was still intact, but backbond oxidation did occur. Above ∼250 °C the hydrogen termination layer was no longer evident in FTIR and considerable oxidation occurred, suggesting reaction or dissociation of the hydrogen layer. This corresponds with an exothermic peak shown during DSC at 300 °C. Thermogravimetric analysis/mass spectroscopy (TGA/MS) was also performed, and confirmed hydrogen gas release beginning at ∼280 °C. A DSC peak at ∼400 °C is evident for fresh samples, but is greatly reduced or not evident for all aged samples. We attribute this peak to backbond oxidation, which is shown to occur in FTIR for all aged samples. Variable heating rate DSC experiments were also performed to determine activation energy of fresh and aged samples. Activation energy was calculated using the Kissinger Method for the first two exothermic peaks in DSC experiments. For the first peak, corresponding to hydrogen desorption (∼300 °C), activation energy for fresh and aged samples was 132.1 kJ/mol and 132.7 kJ/mol, respectively. The activation energy of the second exothermic peak, corresponding to backbond oxidation, for fresh and aged samples was 183.8 kJ/mol and 159.6 kJ/mol, respectively. Device failure during accelerated aging tests was also used to predict the mean lifetime of porous silicon/sodium perchlorate at room temperature (25 oC) as 100 years with a 90% confidence interval of 31 to 328 years.

Non-isothermal Characterization of the Precipitation Hardening of a Cu-11Ni-19Zn-1Sn Alloy

The precipitation hardening of a Cu-11Ni-19Zn-1Sn alloy has been studied by means of Differential Scanning Calorimetry (DSC), High-Resolution Transmission Electron Microscopy (HRTEM), and hardness measurements. The calorimetric curves, in the range of temperatures analyzed, show the presence of one exothermic reaction followed by an endothermic one. The exothermic DSC peak is due to the segregation of Cu2NiZn precipitates and it is associated to a noticeable improvement of the mechanical properties of the alloy. The endothermic effect is associated to the dissolution of the Cu2NiZn precipitates into the copper matrix for restoring the starting Cu-11Ni-19Zn-1Sn homogeneous solid solution. The reaction mechanisms of these processes have been proposed from the kinetic analysis of the exothermic and endothermic DSC signals. The results obtained point out that tin plays a decisive role on the precipitation hardening of the alloy, because age hardening is not observed in the case of a Cu-Ni-Zn ternary alloy of similar composition.

ТЕРМИЧЕСКИЙ АНАЛИЗ ДРЕВЕСИНЫ ЛИСТВЕННИЦЫ (LARIX GMELINII (RUPR.) RUPR.)

The thermal decomposition of tree rings (separately, latewood and earlywood) of Larix gmelinii (Rupr.) Rupr.) during the period from 1988 to 1998 was studied using thermogravimetric analysis (TG / DTG) and differential scanning calorimetry (DSC). Thermal analysis was performed in oxidizing (air) condition. The stages of thermal decomposition of wood were analyzed by heating the sample from 30 to700 °C at the heating rates of 10, 20, 40 °C/min for TG / DTG and from 30 to590 °C at the heating rates of 10, 40 °C/min for DSC. The temperature ranges, mass loss, mass loss rate, temperature DTG / DSC peaks, thermal evaporation effects of moisture and the processes of thermal decomposition for each annual layer were studied. The result of thermogravimetry measurements were carried out using the Broido and Ozawa – Flynn – Wall methods. Tree rings of larch wood on the basis of the analysis of the activation energy values of the individual stages of thermal decomposition and activation energy dependency on the degree of conversion of wood material different tree rings; and based on the comparison of the mass loss for corresponding stages of thermal destruction, thermal effects, and other parameters of TG / DSC and DTG were characterized. The material presented in the study would, in our view, to study the impact of growing conditions on wood physical properties and chemical composition of wood, which are the basis for determining the direction of ways to use it, as well as indicators of the reaction of wood plants on endogenous and exogenous conditions.

Effect of GGBS and curing temperature on microstructure characteristics of lightweight geopolymer concrete

Cement replacement by supplementary cementitious materials has been gaining momentum as a sustainable mechanism to reduce greenhouse gas emissions while also recycling industrial by-products. This paper presents the development and microstructure characterization of fly ash-based lightweight geopolymer concrete incorporating ground granulated blast furnace slag (GGBS). Concrete samples were prepared with 0%, 25% and 50% GGBS replacement and cured at 30°C, 60°C, and ambient temperature. While dune sand and lightweight expanded clay were used as aggregates, a mixture of sodium silicate and sodium hydroxide served as the alkaline activation solution. Microstructure evaluation was carried out at 7 and 28 days employing scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and differential scanning calorimetry (DSC). Residual fly ash and GGBS were identified in the concrete and bonded to geopolymeric reaction products. The microstructure highlighted the formation and coexistence of aluminosilicate hydrate and aluminum-rich calcium silicate hydrate with traces of sodium. Subsequent polymerization was also verified by an increase in FTIR and DSC peaks.

Reference material for temperature calibration of differential scanning calorimeters above 1400 °C

Platinum crucible pans are widely used for differential scanning calorimetry (DSC) at temperatures above the aluminum melting point (about 660 °C) due to good signal quality, chemical inertness and easiness of cleaning. However, reference materials commonly used for the calibration of DSC equipment operating with platinum pans exhibit phase transition temperatures no higher than about 1000 °C. In this work, the solid–solid, reversible, $$\alpha ^{\prime }_{\mathrm{H}}\rightarrow \alpha$$ phase transition of calcio-olivine, $$\hbox {Ca}_{2}\hbox {SiO}_{4},$$ was found to produce a marked DSC peak with an onset temperature of $$1453^{+1}_{-2}\,^{\circ }\hbox {C}$$ and a relatively small hysteresis. This compound is compatible with platinum crucibles and fulfills the requirements to be used as reference material for high-temperature calibration of differential scanning calorimeters.

Comparison of the mineral oil lifetime estimates obtained by differential scanning calorimetry, infrared spectroscopy, and dielectric dissipation factor measurements

In this study, improved observables and new endpoint criteria were developed to assess the remaining useful life of mineral transformer oil using differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR). The tested oil was exposed to thermal ageing at temperatures of 110, 120 and 130°C for times ranging from 100 to 2400h. The intensity of the infrared spectral band of the low-temperature inhibitor and the temperature of the thermo-oxidative DSC peak were considered for evaluation. The obtained results were correlated with standardized dielectric dissipation factor (tan δ) measurements. The results indicated that the analysed observables changed continuously during the applied thermal ageing. The endpoint criteria were subsequently determined and Arrhenius diagrams were constructed. The results demonstrated that the determination of the actual state or the lifetime of the transformer oil via DSC or FT-IR may be beneficial in terms of reducing the measurement time, the influence of moisture on the measurement results and the oil volume required for the tests. Thus, DSC and FT-IR represent promising alternatives to dissipation factor measurements.

High temperature thermal stability of nanocrystalline 316L stainless steel processed by high-pressure torsion

Differential scanning calorimetry (DSC) was used to study the thermal stability of the microstructure and the phase composition in nanocrystalline 316L stainless steel processed by high-pressure torsion (HPT) for ¼ and 10 turns. The DSC thermograms showed two characteristic peaks which were investigated by examining the dislocation densities, grain sizes and phase compositions after annealing at different temperatures. The first DSC peak was exothermic and was related to recovery of the dislocation structure without changing the phase composition and grain size. The activation energies for recovery after processing by ¼ and 10 turns were ~163 and ~106kJ/mol., respectively, suggesting control by diffusion along grain boundaries and dislocations. The second DSC peak was endothermic and was caused by a reverse transformation of α’-martensite to γ-austenite. The hardness of annealed samples was determined primarily by the grain size and followed the Hall–Petch relationship. Nanocrystalline 316L steel processed by HPT exhibited good thermal stability with a grain size of ~200nm after annealing at 1000K and a very high hardness of ~4900MPa.

Curing Mechanism Study for Dual Cure of Epoxy Adhesive by Differential Scanning Calorimetry

Epoxy adhesive used in electronic packaging could normally be cured by ultraviolet light, heat at high temperature or dual cured by both processes. Differential scanning calorimetry (DSC) has been used to identify and analyze the occurred reaction during the curing process. The structural modification of epoxy during curing could be examined by measuring its thermal properties, and the change in molecular structure of epoxy could be observed by a relative small area of DSC peak. This provided the heat amount required for complete cure. It is found that the DSC peak area after heat cure at 90 °C increased linearly as a function of heating time while that at 120 °C decreased exponentially. For UV cure, it indicated that the curing mechanism was strongly depend on the energy from UV light. For dual cure at 90 °C, the heat curing time could be reduced from single curing process of 50 minutes to 6 minutes, while the heating time for dual cure at 120 °C could be reduced from 4 minutes to 2 minutes.

Thermal and spectral characterization of anaerobic thermal behavior patterns in a lacustrine sediment core.

The thermal evolution of sedimentary organic matter is a significant mechanism in continental oil and gas formation. This study presents a new method to estimate vertical thermal evolution trends in a lake sediment core. Twenty sediment samples from a 60-cm core recovered from Lake Bosten were heated to 600°C at a rate of 10°Cmin(-1) under a N2 atmosphere. The sediments were characterized by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), and then, the samples were analyzed with total organic carbon (TOC) analyses, X-ray diffraction, and (137)Cs isotopic dating techniques. Two main anaerobic thermal degradation processes were observed in the thermograms. The pyrolysis results showed variations with sediment age, with labile carbon (237.2 ± 42.98°C) manifesting different thermogram patterns than recalcitrant carbon (498.35 ± 30.09°C). There was a significant linear correlation between sample weight loss and TOC (r = 0.972, p < 0.001), as well as between the DSC and TGA peaks (r = 0.963, p < 0.001). As a conclusion, the thermal stability of both labile organic carbon and recalcitrant organic carbon in lacustrine sediment core increased gradually with age. These results confirm that advanced thermal techniques (DSC and TGA) operated in inert gas are potential quantitative methods to characterize the anaerobic thermal behavior of sediment organic carbon.