Surface Oxidation and Subsurface Microstructure Evolution of Alloy 690TT Induced by Partial Slip Fretting Corrosion in High-Temperature Pure Water

doi:10.1007/s40195-020-01134-9

Abstract

Abstract:

The surface oxidation and subsurface microstructure evolution of Alloy 690TT can occur during partial slip fretting corrosion in high-temperature pure water. Detailed characterization methods such as laser scanning confocal microscopy, scanning electron microscopy, electron probe micro-analyzer, and transmission electron microscopy were used to reveal the related mechanism. The results showed that Cr₂O₃ oxides together with a small number of spinel oxides were formed in sticking region since a small quantity of high-temperature water could pass through the gaps between the asperities to oxidize the materials. Widespread distribution of oxides in microslip region consisted of (Ni, Fe)Cr₂O₄, because Ni²⁺ and Fe²⁺ ions could react with Cr₂O₃ to generate a small amount of non-stoichiometric spinel oxides. The oxides around micropitting in microslip region consisted of double-layer structure. The outermost layer contained (Fe, Cr)-rich oxides due to the effect of fretting leading to mechanical mixing between Cr₂O₃ and (Ni, Fe)(Fe, Cr)₂O₄. The inner layer consisted of (Fe, Ni)-rich oxides owing to the consumption of Cr₂O₃ by the reaction with Ni²⁺ and Fe²⁺ ions. The reciprocating motion of oxide particles in microslip region resulted in the stress-strain supporting the recrystallization for the formation and development of a tribologically transformed structure in subsurface and plowing effect by fretting in surface.

Key words: Fretting corrosion, Oxidation, Partial slip, Alloy 690TT, Microstructure, High-temperature water

Long Xin, Yongming Han, Ligong Ling, Yonghao Lu, Tetsuo Shoji. Surface Oxidation and Subsurface Microstructure Evolution of Alloy 690TT Induced by Partial Slip Fretting Corrosion in High-Temperature Pure Water[J]. Acta Metallurgica Sinica (English Letters), 2021, 34(4): 543-554.

Figures/Tables 13

Table 1 Chemical compositions of alloys (wt %)

Specimen	Ni	Fe	Cr	C	Ti	Mn	Si	P	S
Alloy 690TT	Bal.	11.6	29.9	0.025	0.33	0.25	0.33	0.086	0.0025
Type 304SS	9.35	Bal.	18.3	0.018	-	1.31	0.31	0.034	0.0025

Fig. 1 Schematic diagram of a the water loop, b the configuration of fretting test rig

Table 2 Fretting test conditions and water chemistry parameters

Normal load	Displacement amplitude	Frequency	Duration time	Temperature	Pressure	PH	DO
100 N	60 μm	30 Hz	2 h	288 °C	8.3 MPa	5.6	2 ppm (by weight)

Fig. 2 a LSCM morphology of wear scar on Alloy 690TT after fretting corrosion in HTHP water, b cross-sectional profile of the wear scar with the value of measured wear volume, c EPMA-line scanning analysis for the oxygen concentration on worn surface

Fig. 3 a Magnified SEM morphology of central sticking region of wear scar on Alloy 690TT and b corresponding Raman analysis of the oxide film in the red circle in a

Table 3 Wavenumber corresponding to the typical oxides for Ni-Fe-Cr alloys in Raman spectra

Oxides	Kim et al. [23]	Kim et al. [24]	Maslar et al. [25,26,27]	Wang et al. [28]	Xiao et al. [29]	Miyazawa et al. [30]	Mstsuda et al. [31]
NiO		1074
		910
		725
	480	532	490
Cr₂O₃	608	610	613
	550	550	552
		528	527
	347	352	350
	302	302	300
NiFe₂O₄	695	702	705
	650	654	655
		595	592
	565	574	570
	488	492	488
	455	460	457
	325
NiCr₂O₄				796
	665	687	686	686
				580
	549	550-560
	508	513	512	511
	425	429		425
	325
				181
FeCr₂O₄						683	681
						590	600
						492
Fe₃O₄			665		661
			524		532
			292		300
Fe₂O₃			1310		1320
			1100
			1055
			813
			655
			607		613
			494		498
			406		412
			290		293
			243		247
			224		225

Fig. 4 a Typical SEM-SE2 morphology of microslip region of wear scar in Alloy 690TT, (b) magnified SEM-InLence morphology taken from the rectangle in a, c typical SEM-InLence morphology showing the oxide distribution

Fig. 5 EDS point analysis results for the oxide particle a 1 and b 2 in Fig. 4c

Fig. 6 Raman analysis for the selected worn surface of Alloy 690TT after fretting corrosion in HTHP water: a LSCM image showing five locations for Raman test, b indexed Raman spectra of these five tests

Fig. 7 SEM images of microslip region on Alloy 690TT after fretting corrosion in HTHP water showing a the area chosen for extraction by FIB lift-out and b the deposited Pt coating on the selected site. TEM results for c BFTEM image of the cross section extracted using a FIB, d corresponding STEM-HAADF image

Fig. 8 a BFTEM image obtained from the rectangle 1 marked in Fig. 7c with the inserted SAED, b STEM-HAADF image of the rectangle region 2 in Fig. 7d and the corresponding EDS elemental mapping of Fe, Ni, Cr and O and quantified EDS results on c point 1 and d point 2 marked in b

Fig. 9 a BFTEM image obtained from the rectangle 3 marked in Fig. 7c, b, c SAED patterns from locations 1 and 2 in a, respectively, d, e corresponding DFTEM images obtained from different diffraction spots in c, respectively, f measured distribution of grain size in oxide layer

Fig. 10 a STEM-HAADF image of the rectangle 4 marked in Fig. 7d, b-f corresponding EDX elemental mappings of Fe, Ni, Pt, Cr and O and g EDX profiles for line scan across the wear debris layer. The arrow in a indicates the location and direction of the composition measurements

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