• Vol 9, No 2 (2018)
  • Electrical, Electronics, and Computer Engineering

The Effect of Oxidative Heat Treatment on the Preparation of Stainless Steel 304 and 316 as the Effective Catalytic Substrate for Carbon Nanotube Growth

Praswasti Wulan , Yuni Lestari

Cite this article as:
Wulan, P.P.D.K., Lestari, Y., 2018. The Effect of Oxidative Heat Treatment on the Preparation of Stainless Steel 304 and 316 as the Effective Catalytic Substrate for Carbon Nanotube Growth. International Journal of Technology. Volume 9(2), pp. 353-363
Praswasti Wulan Chemical Engineering Departement University of Indonesia
Yuni Lestari Chemical Engineering University of Indonesia
Email to Corresponding Author


Stainless Steel (SS) is the potential substrate in Carbon Nanotube (CNT) synthesis; Iron (Fe) and Nickel (Ni) content make SS function doubly as substrate and catalyst. In this study, SS is prepared with chloride acid, HCl (37.8%) and oxidative heat treatment (OHT) at 850oC for 30 minutes. This study aims to identify the effect of OHT on SS in CNT’s formation. The identification is done by using carbon sources of acetylene and camphor. The substrate of SS 304 is varied into foil, plate and wire mesh. The result of using acetylene for 20 minutes in respect of the three variations produces carbon loss of over 90%. This is due to an increase in the Cr percentage which inhibits the formation of the catalyst’s nanoparticles. With the help of ferrocene foil substrate, plate, and wire mesh, the CNT produced are 0.0573 gram, 0.0701 gram, and 0.1246 gram along with a reduction in carbon loss to 30%. The use of the substrate of SS 316 with lower Cr content and additional time of synthesis to 60 minutes yields the mass of 0.6325 gram and carbon loss of 2.76%. By using camphor for 60 minutes, the identification results in an increase of CNT mass in SS 304 of 0.831 for foil, 1.856 for plate and 2.6305 for wire mesh. Scanning Electron Microscopy-Energy Dispersive X-Ray Spectroscopy (SEM-EDX) is used to identify the carbon form on the surface of the SS while Gas Chromatography Flame Ionization Detector (GC-FID) is used to identify the acetylene decomposition. Based on this experiment, SS 304 and 316 type along with the OHT preparation method can be used easily as an effective substrate to produce CNT.

Acetylene; Camphor; Carbon Nanotube; Oxidative heat treatment; Stainless steel


Back in 1991, Ijima discovered carbon with a tubular structure was discovered by which from then, until today has been, known as Carbon Nanotube (CNT). Ever since its discovery, the number of research studies on CNT has increased in relation to the method of synthesis, characteristic, and application. Commercial CNT applications include one of the components of nano-tech electronic equipment such as sensors, semiconductors, and fuel cell (Seah et al., 2011).

A quick process of adsorbing and desorbing hydrogen on CNTs is very useful for storing fuel hydrogen (Sudibandriyo et al., 2015). Recently, Stainless Steel (SS) has become widely used as a substrate for CNT growth in different forms like plate (Camilli et al., 2011) and wire mesh (Sano et al., 2012). In a previous study, substrates were used with ultrasonification preparation (Alves et al., 2012), and the heat treatment included oxidation and reduction steps (Sano et al., 2012) for better CNT alignment. SS contains Fe and Ni that can function both as substrate and catalyst. In order to function as a catalytic substrate, the SS’ surface needs to be prepared to produce a suitable condition for the formation of CNT (Zhuo et al., 2014).

OHT is used as a preparation method combined with acid treatment for chromium reduction in SS 304 and 316.  A recent study showed that both SS 304 and 316 could be used as a substrate for CNT. In this experiment, both substrates were used with the same preparation methods in order to identify their effects on the formation of CNT.

OHT is an oxidation preparation with the presence of oxygen used to increase the reactivity of the substrate and the catalytic area for the formation of CNT (Zhuo et al., 2014). Process is initiated by oxygen dissolution on the SS’ surface until its saturation point at high temperature. Then, the oxygen is diffused to the alloy by the effect of the concentration gradient. Inside, oxygen reacts with the alloy, yielding an oxide substance that is precipitated on the surface (Wulan & Wijardono, 2017). The purpose of this treatment is to destroy slippery coating layers on the SS so that nanocarbon can grow more easily (Wulan & Cendana, 2016). Another advantage of using SS is that it is obtainable and available with various geometries such as plate, foil, and wiremesh. In addition, the use of SS as a substrate can facilitate the direct interaction between CNT and conductive substrate and increase the level of electrical conductivity.

This study was conducted in order to examine the effect of the OHT preparation method on SS 304 and 316 by using carbon sources of acetylene and camphor. The use of acetylene is based on its high reactivity and its effectiveness. Camphor is a renewable carbon source that can be used as a raw material for synthesizing CNT. Camphor is a substance that can be found on the Cinnamomum camphora tree. Therefore, with xylene as the dominant fraction, camphor is the potential alternative carbon source for the formation of CNT (Wulan & Silaen, 2017).

Experimental Methods

In this section, we explain the theoretical basis that informed the present research study, CNT can be produced by using various methods like pyrolysis (Wulan & Wijardono, 2017), plasma enhanced chemical vapor deposition, PECVD, (Teo et al., 2003) chemical vapor deposition, CVD, (Baddour et al., 2008) and floating catalyst chemical vapour deposition, FC-CVD (Wulan and Silaen, 2017). In order to identify the effect of substrate preparation, CNT was produced by using chemical vapour deposition and floating catalyst as the most simply method (Seah et al., 2011).  In this study, SS 304 and 316 was used as substrates for the growth of CNT. The SS preparation method included: ultrasonic process with acetone (95%) for 30 minutes etching with HCl (merck) 37.8% for 10 minutes and OHT at 850oC for 30 minutes.

The synthesis process was carried out at 800oC. The synthesis was undertaken by using acetylene with purity 99%, argon (99%) with the flow rate of 450 sccm, acetylene 40 sccm, and hydrogen (99%) 150 sccm, the synthesis lasted for 20 minutes and 60 minutes. The floating catalyst method was carried outby using 100 mg of ferrocene from sigma aldrich. Camphor synthesis was performed by using 10 grams of camphor for 60 minutes with the flow rate of 100 sccm for argon and 50 sccm for hydrogen. The substrate of the synthesis was weighed in order to determine the number of CNT formed which, then, were stored for the characterization process.

Characterization of SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray Spectroscopy) was used to identify the morphology of the formed CNT. In addition, GC-FID (Gas Chromatography Flame Ionization Detector) was used to identify the compositionof output gas of reactor in order to determine the percentage of carbon loss. The characterization, performed in this study, was SEM JEOL JSM-6510LA Analytical Scanning Electron Microscopy and GC-FID (Flame Ionization Detector) Agilent Technologies 6890N by using capillary dimethyl polisiloxane column.


The results show an OHT loss of over 90% with an increase in the percentage of chromium mass. This was achieved with the help of ferrocene CNT produced with the mass of 0.0573 gram (foil), 0.0701 gram (plate), and 0.1246 gram (wire mesh) along with the reduction in carbon loss of for more than 30%. The use of SS 316 with lower Cr content and additional times of synthesis up to 60 minutes yielded a mass of 0.6325 gram and carbon loss of 2.76%. The use of Camphor as an alternative carbon source resulted within 60 minutes in an increase of CNT mass in SS 304 (0.831 gram for foil, 1.856 gram for plate, and 2.6305 gram for wire mesh).  Xylene and oxygen played a significant role in reducing impurity and increasing the mass of CNT. This was because they served as an oxidizer to ensure that the catalytic substrate remained active. Consequently, CNT had better quality when produced by using Camphor as a source of carbon.


The authors acknowledge the financial support received from Directorate of Research and Community Service Universitas Indonesia under PITTA grant 2017 contract number: 825/UN2.R3.1/HKP.05.00/2017. We are thankful, also, to Laboratory of Chemical and Resource Product Engineering (RPKA) Department of Chemical Engineering, Universitas Indonesia, Laboratory of Lemigas, and Laboratory of Fire and Safety Universitas Negeri Jakarta for the instruments characterization.

Supplementary Material
R2-CE-1043-20180128151013.pdf Supplementary files (1)
R2-CE-1043-20180128151039.pdf Supplementary files (2)

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