Adhesion of Oxides Grown in Supercritical Water on Selected Austenitic and Ferritic/Martensitic Alloys

2017 ◽  
Vol 3 (2) ◽  
Author(s):  
D. Artymowicz ◽  
C. Bradley ◽  
B. Xing ◽  
R. C. Newman

A series of austenitic alloys (800H, H214, I625, 310S, and 347) with different surface finishes were exposed to supercritical water (SCW) at 550 °C and 2.5 × 107 Pa for 120 h, 260 h, and 450 h in a static autoclave with an initial level of dissolved oxygen of 8 ppm. Indentation with a hardness indenter was used for assessment of oxide adhesion. This was compared with the results of a similar test on SCW-oxidized ferritic alloys. Delamination in all the tested ferritic alloys was insufficient for quantification of the results but allowed for qualitative comparison within this group. In the set of austenitic alloys, oxide on stainless steel (SS) 347 exfoliated during cooling from 550 °C, and from the remaining four alloys, only oxide on H214 delaminated, which made the qualitative comparison across the whole group impossible. Energy dispersive X-ray spectroscopy (EDX) revealed that under delaminated external Cr2O3 on H214 alloy, there was a submicron thick layer of Al-rich oxide. To investigate a possible oxide spallation on austenitic samples during exposure, mass loss obtained through descaling was compared with mass gain due to SCW exposure. The results indicated that the applied descaling procedure did not, in most cases, fully remove the scale. Apart from one case (SS 347 with alumina surface finish), there was no clear indication of oxide spallation.

2017 ◽  
Author(s):  
Younghee Lee ◽  
Daniela M. Piper ◽  
Andrew S. Cavanagh ◽  
Matthias J. Young ◽  
Se-Hee Lee ◽  
...  

<div>Atomic layer deposition (ALD) of LiF and lithium ion conducting (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloys was developed using trimethylaluminum, lithium hexamethyldisilazide (LiHMDS) and hydrogen fluoride derived from HF-pyridine solution. ALD of LiF was studied using in situ quartz crystal microbalance (QCM) and in situ quadrupole mass spectrometer (QMS) at reaction temperatures between 125°C and 250°C. A mass gain per cycle of 12 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH<sub>3</sub>)<sub>3</sub> as a reaction byproduct instead of HMDS at 150°C. LiF ALD showed self-limiting behavior. Ex situ measurements using X-ray reflectivity (XRR) and spectroscopic ellipsometry (SE) showed a growth rate of 0.5-0.6 Å/cycle, in good agreement with the in situ QCM measurements.</div><div>ALD of lithium ion conducting (AlF3)(LiF)x alloys was also demonstrated using in situ QCM and in situ QMS at reaction temperatures at 150°C A mass gain per sequence of 22 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C. Ex situ measurements using XRR and SE showed a linear growth rate of 0.9 Å/sequence, in good agreement with the in situ QCM measurements. Stoichiometry between AlF<sub>3</sub> and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF<sub>3</sub>)(LiF)x alloy consists of aluminum, lithium and fluorine. Carbon, oxygen, and nitrogen impurities were both below the detection limit of XPS. Grazing incidence X-ray diffraction (GIXRD) observed that LiF and (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film have crystalline structures. Inductively coupled plasma mass spectrometry (ICP-MS) and ionic chromatography revealed atomic ratio of Li:F=1:1.1 and Al:Li:F=1:2.7: 5.4 for (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film was measured as σ = 7.5 × 10<sup>-6</sup> S/cm.</div>


Coatings ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 379
Author(s):  
Domagoj Mudronja ◽  
Frederik Vanmeert ◽  
Stjepko Fazinic ◽  
Koen Janssens ◽  
Darko Tibljas ◽  
...  

Stone monuments and buildings are susceptible to weathering. Carbonate-based stones are especially vulnerable in acidic environments, whereas magmatic acidic stones are more susceptible to chemical weathering in basic environments. To slow down surface corrosion of limestone and marble artworks/buildings, protective coatings which inhibit calcite dissolution have been proposed. In this work, samples from two stone types with different porosity were treated with ammonium oxalate (AmOx) to create a protective layer of calcium oxalate (CaOx) using the previously developed brushing method. Two different synchrotron microscopy experiments were performed to determine its protective capability. X-ray powder diffraction (SR-μ-XRPD) in transmission geometry allowed visualization of the distributions of calcium carbonate and oxalates along the sample depths. In a second step, X-ray fluorescence (SR-μ-XRF) was used to check the efficiency/integrity of the protective surface coating layer. This was done by measuring the sulfur distribution on the stone surface after exposing the protected stones to sulfuric acid. XRPD showed the formation of a protective oxalate layer with a thickness of 5–15 µm on the less porous stone, while a 20–30 µm thick layer formed on the more porous stone. The XRF study showed that the optimal treatment time depends on the stone porosity. Increasing the treatment time from 1 to 3 h resulted in a decreased efficiency of the protective layer for the low porosity stone. We assume that this is due to the formation of vertical channels (cracks) in the protective layer.


CORROSION ◽  
10.5006/3881 ◽  
2021 ◽  
Author(s):  
Zachary Karmiol ◽  
Dev Chidambaram

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.


2019 ◽  
Vol 66 (2) ◽  
pp. 236-241 ◽  
Author(s):  
Somrerk Chandra-Ambhorn ◽  
Neramit Krasaelom ◽  
Tummaporn Thublaor ◽  
Sirichai Leelachao

Purpose This study aims to apply the pack cementation to develop the Fe-Al layers on the surface of FC 25 cast iron in order to increase the high-temperature corrosion resistance of the alloy. Design/methodology/approach Pack cementation was applied on the surface of FC 25 cast iron at 1,050°C. The bare and aluminised alloys were subjected to the oxidation test in 20 per cent O2-N2 at 850 °C. Scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy and X-ray diffraction (XRD) were used for characterisation. Findings The layers of pack cementation consisted of Fe2Al5, FeAl2 and FeAl, and solid solution alloyed with Al. The oxidation kinetics of the bare cast iron was parabolic. Mass gain of the aluminised cast iron was significantly decreased compared with that of the bare cast iron. This was because of the protective alumina formation on the aluminised alloy surface. Al in the Fe–Al layer also tended to be homogenised during oxidation. Originality/value Even though the aluminising of alloys was extensively studied, the application of that process to the FC 25 cast iron grade was originally developed in this work. The significantly reduced mass gain of the aluminised FC 25 cast iron makes the studied alloy be promising for the use as a valve seat insert in an agricultural single-cylinder four-stroke engine, which might be run by using a relatively cheaper fuel, i.e. LPG, but as a consequence requires the higher oxidation resistance of the engine parts.


1999 ◽  
Vol 17 (2) ◽  
pp. 217-224 ◽  
Author(s):  
T.R. DITTRICH ◽  
S.W. HAAN ◽  
M.M. MARINAK ◽  
D.E. HINKEL ◽  
S.M. POLLAINE ◽  
...  

Several choices exist in the design and production of capsules intended to ignite and propagate fusion burn of the deuterium–tritium (D–T) fuel when imploded by indirect drive at the National Ignition Facility (NIF). These choices include ablator material, ablator dopant concentration and distribution, capsule dimensions, and X-ray drive profile (shock timings and strengths). The choice of ablator material must also include fabrication and material characteristics, such as attainable surface finishes, permeability, strength, transparency to radio frequency and infrared radiation, thermal conductivity, and material homogeneity. Understanding the advantages and/or limitations of these choices is an ongoing effort for LLNL and LANL designers. At this time, simulations in one-, two-, and three-dimensions show that capsules with either a copper-doped beryllium or a polyimide (C22H10N2O4) ablator material have both the least sensitivity to initial surface roughnesses and favorable fabrication qualities. Simulations also indicate the existence of capsule designs based on these ablator materials which ignite and burn when imploded by less than nominal laser performance (900-kJ energy, 250-TW power, producing 250-eV peak radiation temperature). We will describe and compare these reduced-scale capsules, in addition to several designs which use the expected 300-eV peak X-ray drive obtained from operating the NIF laser at 1.3 MJ and 500 TW.


2014 ◽  
Vol 809-810 ◽  
pp. 43-52
Author(s):  
Hua Hua Wang ◽  
Nan Li ◽  
Kai Li ◽  
Yuan Bu ◽  
Wen Le Dai ◽  
...  

Multiwalled carbon nanotubes (MWCNTs) as an excellent supporter covered with a thick layer of cobalt phthalocyanine (CoPc) were prepared by in-situ synthesis. Platinum particles were adopted to enhance the conductivity of CoPc-MWCNTs. The final nanocomposite Pt-CoPc-MWCNTs was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Strong aromatic π-π stacking between MWCNTs and CoPc made CoPc in-situ forming on MWCNTs. With homogeneous thickness of CoPc covered on the MWCNTs and Pt particles equally distributed, the nanocomposite was used as electrocatalyst. The electrochemical properties of the composite got researched by casting the dispersion of Pt-CoPc-MWCNTs on the glassy carbon electrode. Compared with other modified electrodes, Pt-CoPc-MWCNTs/GC electrode exhibited excellent electrochemical activity towards dopamine (DA) and uric acid (UA). Linear responses for DA and UA were obtained in the ranges of 5 to 170 μM and 5 to 100 μM, and limits of detection were 2.6 and 1.4 μM (S/N= 3), respectively. Simultaneous detection of DA and UA in the presence of ascorbic acid (AA) also displayed selective property, with no interference to each other.


Author(s):  
ZHAO ZHANG ◽  
JIANING LI ◽  
ZHIYUN YE ◽  
CAINIAN JING ◽  
MENG WANG ◽  
...  

In this paper, the high-temperature oxidation resistant coating on the TA15 titanium alloy by laser cladding (LC) of the KF110-B4C-Ag mixed powders was analyzed in detail. The scanning electron microscope (SEM) and energy dispersive X-ray spectrometer (EDS) images indicated that a good metallurgy bond between the fabricated coating/TA15 was formed; also the fine/compact microstructure was produced after a cladding process. The oxidation mass gain of TA15 was higher than that of the coating after LC process, which were 3.72 and 0.91[Formula: see text]mg[Formula: see text]cm[Formula: see text], respectively, at 60[Formula: see text]h, greatly enhancing the high temperature oxidation resistance.


2016 ◽  
Vol 107 ◽  
pp. 746-752 ◽  
Author(s):  
Akira Yoko ◽  
Makoto Akizuki ◽  
Naohisa Hirao ◽  
Shinji Kohara ◽  
Mukesh Kumar ◽  
...  

2020 ◽  
Vol 1010 ◽  
pp. 65-70
Author(s):  
Zahraa Zulnuraini ◽  
Noraziana Parimin

This paper investigates the performance of Fe-33Ni-18Cr alloy at high temperature oxidation. The samples were isothermally oxidized at three different oxidation temperatures, namely, 600 °C, 800 °C and 1000 °C for 150 hours. This alloy was ground by using several grits of SiC paper as well as weighed by using analytical balance and measured by using Vernier caliper before oxidation test. The characterization was carried out using scanning electron microscope (SEM) equipped with energy dispersive x-ray (EDX) and x-ray diffraction (XRD). The results show that, the higher oxidation temperatures, the weight gain of the samples were increase. Sample of 1000 °C indicate more weight gain compared to samples oxidized at 600 °C and 800 °C. The kinetic of oxidation of all samples followed the parabolic rate law. The surface morphology of oxide scale at lower temperature is thin and form a continuous layer, while at high temperature, the oxide scale develops thick layer with angular oxide particles.


2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Oleksandr Grynko ◽  
Tristen Thibault ◽  
Emma Pineau ◽  
Gytis Juska ◽  
Alla Reznik

AbstractPolycrystalline Lead Oxide (poly-PbO) was considered one of the most promising photoconductors for the direct conversion X-ray medical imaging detectors due to its previous success in optical imaging, i.e., as an optical target in so-called Plumbicon video pick-up tubes. However, a signal lag which accompanies X-ray excitation, makes poly-PbO inapplicable as an X-ray-to-charge transducer in real-time X-ray imaging. In contrast, the recently synthesized Amorphous Lead Oxide (a-PbO) photoconductor is essentially lag-free. Here, we report on our approach to a PbO detector where a thin layer of a-PbO is combined with a thick layer of poly-PbO for lag-free operation. In the presented a-PbO/poly-PbO bilayer structure, the poly-PbO layer serves as an X-ray-to-charge transducer while the a-PbO acts as a lag prevention layer. The hole mobility in the a-PbO/poly-PbO bilayer structure was measured by photo-Charge Extraction by Linearly Increasing Voltage technique at different temperatures and electric fields to investigate charge transport properties. It was found that the hole mobility is similar to that in a-Se—currently the only commercially viable photoconductor for the direct conversion X-ray detectors. Evaluation of the X-ray temporal performance demonstrated complete suppression of signal lag, allowing operation of the a-PbO/poly-PbO detector in real-time imaging.


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