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Evaluation of the calorific value of exothermic sleeve material by the adiabatic calorimeter

  • Ngo Nhu Hoang , Tsuyoshi Nishi EMAIL logo and Hiromichi Ohta
Published/Copyright: December 6, 2022
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 41 Issue 1

Abstract

Recently, casting simulations have been used to improve the product quality and the yield during casting. However, there are cases in which the simulation results do not reproduce the defects in the product. Although accurate physical property values are necessary for highly accurate simulations, some physical property values are not dependable. Recently, the occurrence of defects, such as shrinkage porosity, has been compared between simulated results and actual products by varying the physical property values given in the simulation. It has been shown that the heat value of the exothermic sleeve in the catalog used to reduce defects may be approximately one-seventh of the actual heating value. In this study, we developed an adiabatic calorimeter with a simple configuration that can realize actual casting conditions. The heat generated by the three types of exothermic sleeves was measured. No difference in calorific value was observed between the three types of samples, and all were approximately 2 kJ·g−1. This value is less than the half of that provided in the catalog.

Keywords: calorific value; thermite reaction; high temperature; exothermic sleeve materials; adiabatic calorimeter; rapid heating condition

1 Introduction

Simulations are used in casting manufacturing to help improve the product quality and the yield in casting processes. Although helpful in many aspects, casting simulation predictions still fail in reproducing actual product defects. Among these defects, shrinkage porosity has a significant impact on reducing the strength of casted metal parts. Thorough knowledge of various physical properties of the used materials is a fundamental prerequisite for accurate simulations. Usually, many physical properties are measured or estimated using reliable procedures to be further used in simulations.

Sleeves are heat-insulating materials in which molten metal is poured into a mold at an elevated temperature. The exothermic sleeve is made by mixing a heat-generating substance via a chemical reaction caused by the increase in the temperature during the molten metal injection. This is intended to maintain the molten metal at high temperatures for longer periods, thereby preventing a large pressure drop owing to flow resistance in the solidifying mush. Ultimately, this process helps improve the soundness of the casting products. The calorific value of an exothermic sleeve is a physical property related to the integrity of the product usually solely available from manufacturers’ catalogs. Nevertheless, the development of reliable methods for measuring the calorific values of the exothermic sleeve to verify manufacturers’ data is of paramount importance for ensuring accurate simulations and hence better final product quality. An exothermic sleeve is an inhomogeneous material containing aluminum chips. Thus, the small amount of sample used for differential scanning calorimetry (DSC) measurement [1] has a large variation in calorific value, and the heating rate of 10 K per minute is slow compared to the rate at which molten metal is poured into the sleeve material. Therefore, the heating value of the sleeve material with respect to casting conditions has not yet been measured. The mechanism of heat generation in exothermic sleeves has not been fully understood yet [2,3,4,5]. Niyama et al. [3] attempted to understand this behavior based on the heat transfer rate in sleeves. They reported multiple exothermic reactions without clear explanations regarding the involved mechanisms and the amount of generated heat.

Ito et al. [6] compared the shrinkage porosities during actual casting to those obtained by simulation for castings with complex shapes. Such shapes are prone to manufacturing defects owing to the decrease in the molten metal flow as its temperature drops. It was shown that many shrinkage porosities were generated in the actual casting process even under the same conditions that produced sound results in the simulations. Interestingly, it was noted that the occurrence of defects was almost identical between the simulation and the actual product when the heating values of the exothermic sleeves were approximately one-seventh of the catalog value of 7.5 kJ·g−1.

In this study, we evaluated the calorific value of exothermic sleeves for casting using calorimetry. An adiabatic calorimeter was developed for this goal.

2 Experimental methods

2.1 Principle

According to the first law of thermodynamics, in absence of energy exchange with its external thermal region, the temperature of a system increases from T 1 to T 2 when a thermal energy Q (i.e. from heat generation) is added to it.

(1) Q = C ( T 2 – T 1 ) = C Δ T ,

where C is the heat capacity of the system and ΔT is the temperature increase. Before measuring the calorific value of the target sample, various known heat quantities Q are provided to the device by electric heating, and the temperature rise ΔT is measured to derive C, which is used to determine Q generated by the sample.

2.2 Adiabatic calorimeter for casting

A schematic of the adiabatic calorimeter is shown in Figure 1. The heating sleeve was cut into 20 mm × 20 mm × 5 mm samples. A nichrome ribbon heater (1.5 mm wide and 0.4 mm thick) was wrapped five times around the sample at equal intervals and set in the center of the device. Alumina fiber bricks of 4 mm thickness were placed around the sample and the nichrome ribbon to prevent damage to the parts around the heating section due to the rapid increase in the temperature. Alumina bricks are thermally and chemically inert up to elevated temperatures and exhibit excellent electrical and thermal insulation properties. The heat generated by the sample slowly transfers through the alumina brick to reach the 5 mm thick brass plates of the calorimeter device. The overall external dimensions of the calorimeter system were 100 mm × 50 mm × 35 mm, and the entire surface of the rectangular body was covered with a 30 mm thick Styrofoam sheet to insulate the device. A 10 V DC voltage was applied to the plug pole to heat the sample. The temperature of the nichrome ribbon increased to 1,200 K in 30 s and ignited the heating sleeve when the heat was measured. The heat in equation (1) is the sum of the amount of heat generated by the heating sleeve and the amount of heat generated by the power supply.

Figure 1 A schematic diagram of the adiabatic calorimeter.
Figure 1

A schematic diagram of the adiabatic calorimeter.

2.3 Measurement of heat generated by the power supply

To measure the amount of heat input from the power supply, the voltage (E) and current (I) were measured. The heat quantity Q e is obtained by integrating IE over time, t. The measurement circuit is shown in Figure 2. When the device was energized, the top lid was opened, and the power supply pole was connected to the power source. When the switch is turned on, the electric current flows through the nichrome ribbon. A data logger recorded the current and voltage every 0.02 s. Power was supplied immediately after the top insulating cover was removed to connect the power cable. The device was then quickly covered again to insulate it from the external environment after being energized.

Figure 2 Power measurement circuit.
Figure 2

Power measurement circuit.

2.4 Calorimeter temperature change

Two thermocouples were connected to the center on the outside of the metal plates, as shown in Figure 2, and temperatures were measured at the front (Point 1) and back (Point 2) of the device. The temperature difference between these two points was about 0.2–0.3 K. The average of the two measured values was used to calculate heat values.

Figure 3 shows an example of the temperature measurement results. Upon energizing, the temperature increased from a start temperature of T min ∼ 290 K to a maximum temperature of T max ∼ 310 K. The temperature rise ΔT (K) is given by:

(2) Δ T = T max – T min .

Figure 3 An example of temperature change. The solid and dashed lines correspond to the temperatures associated at Points 1 and 2, respectively, of the power measurement circuit.
Figure 3

An example of temperature change. The solid and dashed lines correspond to the temperatures associated at Points 1 and 2, respectively, of the power measurement circuit.

The temperature increase, ΔT, was evaluated from the heat capacity of all the components of the apparatus including the sample. However, the heat capacity of the sample could be ignored because the mass of the sample (1.2 g) was smaller than that of the apparatus (837 g). The apparatus constituted components such as alumina layer, nichrome ribbon, and screw. The evaluated heat capacity is explained in Section 2.4.

2.5 Heat capacity of the system

A thermally inert small alumina fiber brick (20 mm × 20 mm × 5 mm in size) was used as a sample without heat generation. The temperature rise was measured by applying a 10 V and varying power feed time. Figure 4 shows the relationship between the input heat and temperature rise, and the good linearity of the measured values. The heat capacity of the apparatus, C, was determined using the least-squares method, assuming a linear relationship Q e = CΔT between the temperature rise ΔT and the input heat Q e, C = 391 (J·K−1). As the mass of the sample brick was 0.7 g, the heat capacity of 0.32 (J·K−1) evaluated from the literature values of specific heat of alumina was sufficiently small compared to the heat capacity of the apparatus, C, to be negligible.

Figure 4 Amount of heat input by the power supply and temperature change.
Figure 4

Amount of heat input by the power supply and temperature change.

2.6 Calorific value of the exothermic sleeve

If the amount of heat generated from the sample is Q s, the following relationship holds:

(3) Q = C Δ T = Q e + Q s .

The heating value Q s of the sample was obtained from equation (3) based on the temperature change ΔT and the input power Q e from the current and voltage during energization.

2.7 Exothermic sleeve material

Table 1 summarizes the composition of the exothermic sleeves of the samples, based on the data provided by the manufacturers [7,8,9]. All exothermic sleeve materials used for samples were commercially available.

Table 1

Composition of exothermic sleeve materials

Composition ratio (mass %)
Sample T Sample F Sample M
Al 20–30 18–23 20–28
Al2O3 15–40 13–23 12–20
SiO2 20–30 28–38 19–25
Fe oxide 5–10(*) 7–12(*) 10–16
Fe2O3 — <1 <2
MgO — — —
CaO <1 — —
Carbon 5–10 — 1–4
Unknown 5–10 4–34 3.5–9.5

(*) Unspecified oxide included.

The heat generated by the sleeve materials is mainly due to the heat of the reaction between aluminum and iron oxide, as shown in equation (4). The thermite reaction occurs at the contact area between aluminum and iron oxide. Then, the progress of the reaction varies depending on the distribution and the grain size of aluminum and iron oxide.

(4) 2 Al + Fe 2 O 3 = Al 2 O 3 + 2 Fe, Δ H ∘ = – 856 kJ .

From equation (4) and the mass per mole of Al and Fe2O3, the weight of iron oxide required for the thermite reaction was three times the amount of aluminum. However, in the composition table (i.e., Table 1), the mass of iron oxide was approximately twice that of aluminum. Thus, all samples have excess aluminum for the thermite reaction in equation (4). In the presence of ambient oxygen, aluminum behaves as an exothermic substance owing to the oxidation reaction, as shown in equation (5). Although this reaction is highly exothermic, the aluminum oxide layer formed on the surface acts as a barrier to the reaction, blocking oxygen and slowing the progress of the reaction under atmospheric conditions.

(5) 2 Al + 3 / 2 O 2 = Al 2 O 3 , Δ H ∘ = − 1 , 674 kJ .

3 Results and discussion

Table 2 lists the measurement results for the various samples. Samples F and M were measured twice, and T was measured four times to confirm reproducibility. The aluminum in our samples was mainly made of chips with sizes ranging from approximately 0.1 to 4 mm, and the content varied between the different samples. Therefore, some variations in the measured values were observed with no significant difference by product type in calorific values. The average heating values for samples F, M, and T were 2,076, 2,021, and 2,079 (J·g−1), respectively.

Table 2

Calorimetry results and calorific values calculated from aluminum and iron oxide content

Physical properties Unit Sample T Sample F Sample M
Temperature, T min K 290.0 294.0 295.0 294.0 292.1 295.4 295.0 296.0
Temperature, T max K 309.8 313.7 315.2 314.1 311.7 314.0 316.4 317.3
Ignition heat, Q e J 5,491 5,355 5,395 5,529 5,398 5,166 6,022 5,537
Sample mass g 1.030 1.127 1.128 1.124 1.054 1.052 1.300 1.300
Measured heat, Q J 7,742 7,664 7,781 7,742 7,664 7,273 8,485 8,328
Sample heat, Q s J 2,251 2,309 2,386 2,213 2,266 2,107 2,463 2,791
Calorific value J·g−1 2,185 2,048 2,115 1,969 2,150 2,003 1,894 2,147
Thermite reaction heat* J·g−1 0,401 0,508 0,696
Al oxidation reaction heat* J·g−1 6,965 5,363 6,706
Total reaction heat* J·g−1 7,366 5,871 6,772

(*) Calculated from chemical composition.

Table 2 also shows the exothermal values when all iron oxides react with aluminum during the thermite reaction, the exothermal values when all aluminum remaining from the thermite reaction reacts with oxygen in the air, and the total exothermal values for these two reactions combined. The contents used in calculations were determined using the median value of the composition range: 20.5% aluminum and 9.5% Fe2O3 for sample F, 24% aluminum and 13% Fe2O3 for sample M, and 25% aluminum and 7.5% Fe2O3 for sample T. The measured values obtained were smaller than the total heat generation obtained by calculation, however larger than the heat generation assuming only the thermite reaction. This shows that the thermite reaction and oxidation of aluminum proceed together.

Ito et al. [6] compared the occurrence and distribution of defects caused by shrinkage and molten metal flow for actual products, and those obtained using the casting simulations system (ADSTEFAN Ver. 2013) [10]. By varying the heat generated by the exothermic sleeve in simulations and matching the defect densities and positions between simulated and real products, they predicted that the heat of the sleeve was approximately 1 kJ·g−1. The experimental results consistently showed that the catalog value of approximately 7.5 kJ·g−1 was excessive.

Incidentally, the value measured by DSC in the air was approximately 3.4 kJ·g−1 [2], which is larger than the value measured in this study. In the DSC measurements, the sample was finely crushed, and its temperature was increased to 1,473 K in 120 min, at a slow rate of 10 °C·min−1 in air, to measure the exothermic value. Under these conditions, the slow but highly exothermic oxidation reaction shown in equation (5) is considered to have progressed considerably. In industry, exothermic reactions occur in the process of rapid heating by molten metal injection and subsequent cooling by heat dissipation to the sand mold. Therefore, the values measured by DSC are not considered to be meaningful for actual operations.

4 Conclusions

The calorific value of the exothermic sleeve material is evaluated using an adiabatic calorimeter. The calorimeter corresponds to the measurement of the actual reaction during the casting process via rapid heating. The obtained values indicate that the calorific values provided in the manufacturer’s catalog are approximately twofold larger than the actual values. These results are consistent with the tendency shown by the numerical simulations for actual casting. The validity of this measurement is confirmed by the fact that highly linear data were obtained in the calibration experiment, which was performed by feeding the measured heat. The measurement method developed here is simple, compact, and inexpensive and is expected to be used for pre-furnace analysis in the casting industry.

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Acknowledgment

We would like to thank Atsutomo Katsumata for his kind support.

  1. Funding information: This work was supported by JSPS KAKENHI (grant number JP19K05107). The results were obtained through joint research between Ibaraki University and Ito Foundry and Machinery Co., Ltd. We would also like to thank the Hitachi Regional Technical Support Center for their support in preparing the apparatus used in this study.

  2. Author contributions: Ngo Nhu Hoang: Data curation, formal analysis, writing original draft, writing review, and editing. Tsuyoshi Nishi: Validation, investigation, writing original draft, writing review, and editing. Hiromichi Ohta: Conceptualization, Methodology, investigation writing review, and editing.

  3. Conflict of interest: Authors state no conflict of interest.

References

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Received: 2022-07-02
Revised: 2022-09-01
Accepted: 2022-09-12
Published Online: 2022-12-06

© 2022 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/htmp-2022-0240
Keywords for this article
calorific value; thermite reaction; high temperature; exothermic sleeve materials; adiabatic calorimeter; rapid heating condition
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