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Article

Experimental Study on Microalloyed Steel with Layers Subjected to Diesel

by
Noé López Perrusquia
1,*,
Tomas de la Mora Ramírez
2,
Gerardo Julián Pérez Mendoza
1,
Víctor Hugo Olmos Domínguez
3,
David Sánchez Huitron
1 and
Marco Antonio Doñu Ruiz
1,*
1
Grupo Ciencia e Ingeniería de Materiales, Universidad Politécnica del Valle de México, Av. Mexiquense s/n, col. Villa Esmeralda, Tultitlán 54910, Mexico
2
Tecnológico de Estudios Superiores de Jocotitlán, Tecnológico Nacional de México, Carretera Toluca-Atlacomulco, Km 44.8, Ejido de San Juan y San Agustìn, Jocotitlán 50700, Mexico
3
Universidad Tecnológica de México—UNITEC-MÉXICO Campus Atizapán, Universidad en Atizapán, Blvrd Calacoaya 7, MZ 012, La Ermita, Cdad. López Mateos 52970, Mexico
*
Authors to whom correspondence should be addressed.
Coatings 2024, 14(7), 912; https://doi.org/10.3390/coatings14070912 (registering DOI)
Submission received: 8 May 2024 / Revised: 9 July 2024 / Accepted: 16 July 2024 / Published: 21 July 2024
(This article belongs to the Special Issue Surface Engineering, Coatings and Tribology)
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Abstract

:
This work studies the mechanical behavior of microalloyed steels (API X60 and API X70) with boride layers using a boriding process and immersion in diesel. First, the microalloyed steels were borided using dehydrated boron paste at a temperature of 1273 K for 6 h, and then the borided microalloyed steels were immersed in diesel for one year. The characterization of the layers on the specimens subjected to diesel used scanning electron microscopy (SEM), energy dispersive spectroscopy, and X-ray diffraction (XRD). The evaluation of the mechanical properties was performed with tensile tests according to ASTM E8, and then the fracture surface was observed by SEM. This work contributes to the understanding of the changes in the mechanical properties of borided microalloyed steel immersed in diesel for possible potential applications in the storage of fuels, oils, hydrogen, and biofuels.

1. Introduction

Actually, the modification of non-ferrous and ferrous materials with coatings has the purpose of generating better performance for the storage and transportation of diesel and oil fuels and their petroleum derivatives, as well as new fuels from grains and organic materials [1,2]. In this new era, the automotive, aeronautical, maritime, marine, and aerospace industries are constantly growing, changing, and innovating to have the option of materials with surface coatings to satisfy industrial needs [3]. The automotive, maritime, agricultural, and aerospace industries, as well as all those that use hydrogen, diesel, oil, and/or biofuels, need innovative materials with a higher working efficiency and less deterioration of their parts and/or engineering components to reduce replacement to make the industries more cost efficient [4,5].
The different ferrous materials exposed to conventional fuels and/or biofuels must be continuously improved to meet the current requirements of each industry, improving the characteristics of the materials to obtain a range of properties to be designed to create engineered products and parts to support the storage and transportation of diesel, oil, hydrogen, and biofuels [6,7,8,9]. In this scenario, with the need to develop materials with coatings for the transport and storage of diesel, oil, hydrogen, and biofuels, companies, governments, and researchers are currently working on generating, modifying, and innovating materials with surface coatings in an intense activity to show the progress obtained in mechanical, physical, and chemical properties [10,11,12,13,14,15,16,17,18,19,20,21].
According to [22], there are three techniques of boriding: boriding in gaseous media, boriding in liquid media, and boriding in solid media. In the case of solid media, which includes paste boriding, the paste contains boron carbide (B4C) and cryolite (Na3AlF6). In previous work [23,24,25], the current trend of dehydrated paste was used in their studies. Boriding has been used for surface and hardness improvement, corrosion resistance, and other processes for numerous materials.
A few reports of the dehydrated paste process on metallic materials have shown a favorable response as a barrier for possible alternative fuel applications [26,27]. However, a range of studies are required on the effect of diesel on materials with boride layers [27,28].
In the present work, the characterization and mechanical properties of each microalloyed steel (API X60 and API X70) with boride layers exposed to immersion in diesel were evaluated. This will give a better appreciation of the effect of the boride layers on these microalloyed steels exposed to diesel, with the possibility of future applications. As such, this will generate research areas for future work on boriding microalloyed steels exposed to different fuels derived from petroleum, biodiesel, oil, and biofuels.

2. Materials and Methods

2.1. Materials

Microalloyed steel grades API-X60 and API-X70 are shown according to composition in Table 1. Following machining, dogbone tensile test specimens were fabricated based on the standard ASTM E8/E8M, as shown in Figure 1.

2.2. Dehydrated Paste Pack Boriding

Dehydrated paste pack boriding was carried out with Durborid© commercial dehydrated boron paste with boron carbide and cryolite [19], and API-X60 and API-X70 steel specimens were subjected to 1273 K with a permanence of 6 h. Then, specimens were removed from the muffle at room temperature. Figure 2 shows the distribution of the specimens in the container for the boriding process and also shows the specimens submitted after the boriding process.

2.3. Microalloyed Boriding Steel Immersed in Diesel

Table 2 shows the experimental condition and codes for each microalloyed steel exposed to diesel, and Figure 3 shows the configuration on borided microalloyed steel subjected to diesel. Seven specimens of each microalloyed steel were introduced into each container. The immersion was subjected to diesel for one year at room temperature, the immersion tests were repeated 4 times, and then the specimens were removed from the container to evaluate the characterization and mechanical properties under tensile test.

2.4. Tensile Testing and Characterization

The tensile testing of the PB60ID and PB70ID specimens was performed on a universal mechanical testing machine Shimadzu model AG-X, with a test speed of 0.15 mm/min, as shown in Figure 4. The characterization of the PB60ID and PB70ID specimens was performed using the metallographic process to obtain the surface microstructure and analyze the type of iron boride by scanning electron microscopy (SEM). The thickness of the boride layers was measured using a digital thickness-measuring instrument attached to the SEM, and the thickness values are averages of at least fifty measurements in five different micrographs. Moreover, the present phases were evaluated using Bruker D8 advanced equipment with CuKα radiation at λ = 1.54 Å. Finally, fractography analyses on PB60ID and PB70ID were performed with SEM to extract the details of the fracture surfaces of each condition.

3. Results and Discussion

3.1. Surface Microstructure of PB60ID and PB70ID

Figure 5 shows the micrographs with the presence of a boride layer formed on the surface of PB60ID and PB70ID; three areas can be observed: the FeB layer on top, the Fe2B layer below the FeB layer, and the substrate with the microstructure of the microalloyed steels. For PB60ID, the thickness of the total layer (FeB + Fe2B) was around of 245.97 ± 15.55 µm and 74.25 ± 12.55 µm for the Fe2B layer, as well as 255 ± 19.55 µm and 82.39 ± 15.55 µm for the total layers and FeB layers, respectively, for PB70ID. During the dehydrated paste pack boriding, redistribution of the alloying element takes place depending on the solubility of the element in the iron boride. Figure 5 shows the EDS analysis in each specimen and allows the identification of the elements Mo, Al, V, Cr, Cu, and Nb, which were dissolved in the FeB/Fe2B bilayer on the PB60ID and PB70ID specimens.
The presence of alloying elements reduces the diffusivity of the boron in the substrate, thus decreasing the thickness of the FeB/Fe2B layers. Figure 5 shows the micrographs of each microalloyed steel with FeB/Fe2B and Fe2B/substrate-layered interfaces with saw-tooth morphology; similar works on low-alloy steels show the saw-tooth morphology of borides [29,30,31]. However, high-alloy steels have a flat interface between the boride layers and substrate [23]. In addition, boriding in solid media, the influence of the formation of boride and thickness is due to the potential of boron, and this process can be carried out by the three boronizing potentials of B4C powder [32], low, intermediate, and high. Dehydrated paste packs have high potential (90% B4C-10% KBF4) that shows the presence of two phases (FeB + Fe2B) in each microalloyed steel, which was also affected by the temperature and time of boriding process [33].
PB60ID and PB70ID showed no alteration in the morphology, failure of the boride layers, and thickness of the FeB/Fe2B bilayer after one year subjected to diesel. In addition, corrosion zones were shown on the substrate for PB60ID and PB70ID, and this was caused by the porosity in the boride bilayers, as evidenced by the results published in the literature [28,34,35]. In contrast, the failure of the FeB and Fe2B layers on AISI H13 after 70 h and 120 h of immersion in H2S04 5vol.% and H3PO4 30 vol.%, respectively, was observed [36].

3.2. XRD of PB60ID and PB70ID

Figure 6a,b show the XRD patterns in PB60ID and PB70ID, respectively, and Table 3 reveals the presence of the FeB and Fe2B phase planes and peaks for PB60ID and PB70ID. Notable for PB60ID was the high peak at 63.00° for FeB, and the peaks at 45.12° and 57.58° were revealed to contain FeB/Fe2B. For PB70ID, the high peak at 37.74° for FeB was notable, but the peaks at 45.10° and 57.58° contained FeB/Fe2B. The XRD results were supported by EDS, as shown in Figure 5a,b, showing the times used are sufficient to obtain the Fe2B/FeB iron boride bilayer. The temperature for PB60ID and PB70ID caused a significant increase in the intensity of the primary FeB peak, as shown in Figure 6.
The results of the XRD patterns evidence the formation of iron boride on the surfaces of PB60ID and PB70ID. Furthermore, it was determined that diesel has no significant effect on determining the iron boride phases in PB60ID and PB70ID. However, it was observed that as the peak intensities increased, the thickness of the boride layer formed on the surface of the material due to the boriding temperature.

3.3. Tensile Test Results (Ultimate Tensile Strength, Yield Strength, and Elongation)

Figure 7 shows the behavior of the stress versus strain curves for PB60ID and PB70ID. The results of the ultimate tensile strength (UTS) and yield strength (YS) values for PB60ID and PB70ID were lower than the values for microalloyed steels in the literature, and these values are present in Table 4.
Specimen PB60ID shows a decrease in YS and UTS compared to PB70ID. In both specimens, the UTS and YS decreased by more than 50% for commercial API X70 [37] and API X60 [38], and the strength was negatively influenced by the presence of the brittle dual borided layer and immersion in diesel for one year.
In the case of boriding, similar results have been obtained by A. Calik et al. [40] for borided pure nickel, where the YS and UTS decreased by increasing the boriding time. L. M. Alcatar Martinez et al. [39] observed that the UTS and YS decreased for API 5L grade B steel with Fe2B layers on the surface. However, according to the standard API 5L [41], which specifies the mechanical characteristics of these steels, the boriding process can be used on pipes and fittings.
On the other hand, there is limited literature on boride layers for applications in the diesel industry. Some work, such as that of Walter Fichtl [42], reports that an engineered part with a boron layer exposed to diesel has significant performance. Mehmet Cakir et al. [43] present a study showing improved efficiency of a boron layer engineering part with diesel interactions. Considering a few studies of boriding microalloyed steels with diesel interactions, this work originated with the PB60ID and PB70ID specimens, contributing to the recent literature and providing an option for the product engineering and international manufacturing processes of these materials. However, the change in mechanical properties depends on the thickness of the boride layer and the effect of temperature, as evidenced in published works [44,45,46].
The limited studies show the mechanical properties of non-ferrous and ferrous materials with different types of coatings and without coatings exposed to diesel or biodiesel [7,8,9,10]. However, the few studies using different boriding processes show changes in mechanical properties on different metallic materials, generating possible applications in biofuel storage and/or environmentally friendly fuels [26,47].

3.4. Fractography on PB60ID and PB70ID

Figure 8 shows the fractography of the PB60ID and PB70ID specimens. In the case of the PB60ID specimens shown in Figure 8a, transgranular-type fractures in the zone of the iron boride layer and dimples were detected in the substrate, and it is seen that the areas toward the substrate were fractured in a ductile manner, whereas the boride layers were fractured in a brittle form. Moreover, flaking and cracking were observed on surface borided layers. The flaking is due to the hard and brittle FeB phase and residual stresses as tension and compression have occurred on duplex borided FeB/Fe2B, as well as the cracking by the underapplied load in the tensile test; these tensions cause cracking of the boride layer and flaking off of the FeB layers. In addition, the rough-looking crack patterns on the surface in the cross-section extend along the surface with sharp traces, as described in [48,49].
Similar behavior was also observed in the PB70ID specimens. However, the flaking and cracking on PB60ID occurs to a lesser degree due to the thickness of the brittle FeB layers. In the work of [50], the influence of FeB layer thickness on the flaking and cracking on the surface of the boriding layers was observed on AISI 304 steel.
There are limited studies of the tension testing of materials exposed to different boriding processes to provide results for the petrochemical industry or pipeline manufacturing industry [39]. Furthermore, the results for the PB60ID and PB70ID specimens can contribute to the design of engineering parts in the fuel and/or biofuel storage industry.

4. Conclusions

In this work, the characterization and mechanical properties of PB60ID and PB70ID have been investigated with the following conclusions:
  • Dehydrated boron paste on specimens PB60ID and PB70ID allowed the formation of an FeB/Fe2B bilayer with saw-tooth morphology. The EDS analysis on PB60ID and PB70ID supports that the alloying elements were pushed in the FeB/Fe2B bilayer, and the XRD shows the predominant phase to be FeB iron boride in both specimens due to the chemical composition of each specimen.
  • Immersion in diesel did not alter the phase structure but showed a significant increase in the intensity of the FeB peaks for PB60ID and PB70ID; also, no deformation of the iron boride formed on the microalloyed surfaces.
  • The mechanical properties showed an increase in the PB70ID specimen compared to the PB60ID specimen. No boride layers failed after one year subjected to diesel. However, the mechanical properties decreased by more than 50% in commercial API X70 and API X60 due to the presence of brittle borided layers and immersion in diesel.
  • At the fracture surface of PB60ID and PB70ID, in the microalloyed steels, the fracture was ductile and the transition areas in the boride layer were brittle fractures.

Author Contributions

N.L.P. selected the research and developed the research in cooperation with M.A.D.R. Methodology was developed in collaboration with T.d.l.M.R. and G.J.P.M. Results and data analysis were contributed by D.S.H. and V.H.O.D. contributed to critically revising the manuscript for important intellectual content and the final version. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Data are contained within the article.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. Geometry and dimensions of the tensile test dogbone specimens.
Figure 1. Geometry and dimensions of the tensile test dogbone specimens.
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Figure 2. Parts involved in the dehydrated paste boriding process: 1. container, 2. boron carbide, 3. specimens, and 4. lid.
Figure 2. Parts involved in the dehydrated paste boriding process: 1. container, 2. boron carbide, 3. specimens, and 4. lid.
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Figure 3. Experimental configuration for PB60ID and PB70ID.
Figure 3. Experimental configuration for PB60ID and PB70ID.
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Figure 4. Tensile tests of PB60ID and PB60ID.
Figure 4. Tensile tests of PB60ID and PB60ID.
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Figure 5. SEM and EDS micrographs of cross-sections of (a) PB60ID and (b) PB70ID.
Figure 5. SEM and EDS micrographs of cross-sections of (a) PB60ID and (b) PB70ID.
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Figure 6. XRD patterns: (a) PB60ID and (b) PB70ID.
Figure 6. XRD patterns: (a) PB60ID and (b) PB70ID.
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Figure 7. Strain–stress curve for PB60ID and PB70ID.
Figure 7. Strain–stress curve for PB60ID and PB70ID.
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Figure 8. Fracture surface obtained in (a) PB60ID and (b) PB70ID.
Figure 8. Fracture surface obtained in (a) PB60ID and (b) PB70ID.
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Table 1. Chemical composition of materials (wt.%).
Table 1. Chemical composition of materials (wt.%).
MaterialsCMnSiPSAlCuCrNiMoVNbTiFe
API-X600.121.050.170.020.0040.0220.250.090.130.0430.0470.0260.002Bal.
API-X700.1251.680.270.0140.0020.0350.0180.030.020.0210.0680.0930.003Bal.
Table 2. Experimental codes of borided specimens in diesel immersion.
Table 2. Experimental codes of borided specimens in diesel immersion.
CodesSpecimenTreatment and Exhibition Conditions
PB60IDAPI-X60Exposed to dehydrated paste at 1273 K for 6 h and immersed in diesel for one year
PB70IDAPI-X70Exposed to dehydrated paste at 1273 K for 6 h and immersed in diesel for one year
Table 3. Phases and planes of PB60ID and PB70ID.
Table 3. Phases and planes of PB60ID and PB70ID.
Specimen2θ Peak
[°]		Plans
FeBFe2B
PB60ID32.52(020)-
37.74(101)-
39.58(120)-
41.23(111)-
45.12(021)(211)
47.81(210)-
54.97(130)-
57.58(211)(310)
63.00(002) max.-
PB70ID31.17--
32.52(020)-
35.33-(200)
37.74(101)-
39.59(120)-
41.23(111)-
45.10(021) max.(211)
47.71(210)-
54.97(130)-
57.58(211)(310)
63.00(002)-
65.03(221)-
Table 4. Experimental values for the tensile tests of PB60ID and PB70ID.
Table 4. Experimental values for the tensile tests of PB60ID and PB70ID.
SpecimenConditionBoride
Layers		Ultimate Tensile Strength (MPa)Yield Strength (MPa)Total Elongation (%)Reference
API X70-----69245815.7[37]
API X60----57748027[38]
API 5L grade B steelPowder pack
1273K-6 h
No immersion		Fe2B493.57312.8323.41[39]
API X70Dehydrated paste pack
Immersion diesel		FeB + Fe2B259.57 ± 12.3163.34 ± 11.523.41 ± 0.12Present study
API X60Dehydrated paste pack
Immersion diesel		FeB + Fe2B276.22 ± 13.5194.22 ± 15.5526.18 ± 0.15Present study
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López Perrusquia, N.; de la Mora Ramírez, T.; Pérez Mendoza, G.J.; Olmos Domínguez, V.H.; Sánchez Huitron, D.; Doñu Ruiz, M.A. Experimental Study on Microalloyed Steel with Layers Subjected to Diesel. Coatings 2024, 14, 912. https://doi.org/10.3390/coatings14070912

AMA Style

López Perrusquia N, de la Mora Ramírez T, Pérez Mendoza GJ, Olmos Domínguez VH, Sánchez Huitron D, Doñu Ruiz MA. Experimental Study on Microalloyed Steel with Layers Subjected to Diesel. Coatings. 2024; 14(7):912. https://doi.org/10.3390/coatings14070912

Chicago/Turabian Style

López Perrusquia, Noé, Tomas de la Mora Ramírez, Gerardo Julián Pérez Mendoza, Víctor Hugo Olmos Domínguez, David Sánchez Huitron, and Marco Antonio Doñu Ruiz. 2024. "Experimental Study on Microalloyed Steel with Layers Subjected to Diesel" Coatings 14, no. 7: 912. https://doi.org/10.3390/coatings14070912

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