Acidic Corrosion Behavior of Slag-free Self-shielded Flux-cored Arc Welding Overlay

Abstract

The corrosion resistance of slag-free self-shielded flux-cored welding overlays with different ferrotitanium (Fe–Ti) additions in 3.5 wt.% NaCl + 0.01 mol/L HCl acidic solution was investigated. The corrosion occurs in the matrix rather than M₇(C, B)₃, M₃(C, B) and TiC in the microstructure of all the welding overlays. The corrosion resistance of hypereutectic welding overlay is decreased when the Fe–Ti addition is increased from 0 wt.% to 12 wt.%. The corrosion resistance of the welding overlay is the lowest since the overlay is a eutectic structure at the Fe–Ti addition of 12 wt.%. The eutectic structure increases the interface of corrosion reaction, which accelerates the corrosion rate and increases the corrosion current. With the Fe–Ti addition increasing from 12 wt.% to 24 wt.%, the corrosion resistance of the welding overlays with hypoeutectic structure is gradually increased, owing to the increase of the proportion of TiC and chromium content in the matrix.

1. Introduction

The technological development of high chromium iron-based alloys is essential in the manufacturing of equipment operating in extreme conditions by incorporating higher quality, longer service life, and lower production costs.^1,2,3) The high-Cr iron-based alloys are generally fabricated by different types of welding, viz. shielded metal arc welding (SMAW),^4,5,6) submerge arc welding (SAW),^7,8) electroslag welding (ESW),^9,10) gas tungsten arc welding (GTAW),^11,12) flux cored arc welding (FCAW),^13,14,15) etc. Among different welding processes, flux cored arc welding has the highest deposition efficiency.^16,17) Recently, the slag-free self-shielded flux-cored wire has been developed with continuity of welding process, high-speed melting without using additional gas shielding. The high chromium iron-based hardfacing alloys fabricated by slag-free self-shielded flux-cored wires exhibited excellent wear resistance because of its high alloy filling into the core.^{17,18,19,20,21)} The addition of deoxidizers such as C, Al, Mg, Mn and Si in the filler metal helped reduce the amount of porosity. Furthermore, the formation of CO gas resulted in the welding pool boiling, thus leading to the absence of weld porosity.²¹⁾

High chromium iron-based hardfacing alloys are mainly employed in mechanical parts submitted to severe wearing. In addition, it also needs more resistance to corrosion when in several aggressive industry environments such as petroleum industry parts.^22,23) It was reported that thermal treatments for cast iron alloys may improve the corrosion resistance.^22,23,24) Moreover, the corrosion resistance of high chromium iron-based hardfacing alloys was dominated by the free chromium content in the matrix and the ratio of volume fraction of carbides to ferrous matrix.^25,26) In this study, varying additions of titanium were added into experimental iron-based self-shielded flux-cored wire and the effects of titanium on the corrosion resistance were investigated.

2. Experimental Procedures

The slag-free self-shielded flux-cored wire was composed of a steel-made outer shell taking on a tubular shape and a flux filling the interior of the outer shell. The chemical composition of the outer shell is shown in Table 1. The flux consisted of ferrotitanium, ferroboron, high carbon ferrochrome, electrolytic manganese, ferrosilicon, graphite and iron powders. The flux filling rate which is defined as the ratio of the mass of the flux filling the interior of the outer shell to the total mass of the wire was 50%. Figure 1 shows the flow chart of manufacture method of slag-free self-shielded flux-cored wire. The outside diameter of the flux-cored wire was 2.4 mm. Different additions of Fe–Ti (containing 30 wt.% Ti and 70 wt.% Fe) adding into core wire was 0 wt.%, 6 wt.%, 12 wt.%, 18 wt.%, and 24 wt.% respectively. The balance was made up of pure iron powders.

Table 1. The chemical composition of the outer shell (wt.%).

C	Si	Mn	S	P	Fe
≤ 0.10	≤ 0.03	0.30–0.55	≤ 0.030	≤ 0.030	Bal.

Fig. 1.

The flow chart of manufacture method of slag-free self-shielded flux-cored wire. (Online version in color.)

Welding overlays were deposited on base plates of dimensions 150 mm × 70 mm × 50 mm using slag-free self-shielded flux-cored wire arc welding. In order to eliminate the effect of dilution of base plates on welding overlays, five layers were deposited. The welding process parameters are shown in Table 2.

Table 2. The welding process parameters.

Welding current (A)	280–340
Arc voltage (V)	28–32
Electrode polarity	Positive
Welding speed (m·min−1)	2.5–3.0
Electrode angle to plate surface (°)	10

The specimens of welding overlays were cut from the surface of the weld overlay, polished and etched with the agent which consisted of 15 mL of 38% hydrochloric acid solution, 3 mL of 68% nitric acid solution, 50 mL H₂O and 3 g ferric chloride. Optical microscopy (OM) and scanning electron microscopy (SEM) were used to analyze the microstructure of the specimens. Secondary electron imaging allowed morphologic description of the worn surfaces, while EDS compositional maps were used to qualitatively describe chemical variations in the microstructure.

The electrochemical corrosion test was carried out by using the Preceton-Versa STAT3 electrochemistry workstation. The software in the electrochemical workstation can automatically measure the electrochemical corrosion. It included potential dynamic polarization, corrosion potential measurement, Tafel curve fitting and AC impedance testing. The data fitting analysis of AC impedance was completed by zsimpwin software.²⁷⁾ The conventional three electrode electrochemical corrosion test cell was used for electrochemical corrosion test. The working electrode, counter electrode and reference electrode are inserted into the test unit, and the maximum solution volume of the cell was 100 ml. The sample to be tested was 10 × 10 × 5 mm welding overlays. The electrochemical test solution was 3.5 wt.% NaCl + 0.01 mol/L HCl, the reference electrode is mercurous sulfate electrode, and the counter electrode was 15 × 15 × 0.3 mm platinum plate. The scanning rate of polarization curve was 0.5 mv/s, and the scanning range was - 0.4 V–1.5 V vs. OCP (open circuit potential) in acidic solution. The AC impedance test parameters ranged from 0.01 Hz to 100000 Hz.

3. Results and Discussion

The OM images of high chromium iron base hardfacing alloy with different addition of titanium is shown in Fig. 2. It can be seen that the surfacing effect is good without defects such as pores, cracks or inclusions. Figure 2(a) in the metallographic diagram, the light white hexagonal structure is primary carbide M₇(C, B)₃, and the peripheral gray and white radial structure is eutectic which consists of M₃(C, B), martensite and retained austenite.¹⁸⁾ The microstructure of Ti-free hardfacing alloy is typical of hypereutectic high chromium cast iron. When the addition of Fe–Ti is 6 wt.%, the gray black quadrilateral phase can be observed (Fig. 2(b)). However, the size and quantity of hexagonal primary carbides decrease gradually since the addition of Fe–Ti reaches 12% (Fig. 2(c)). As the addition of Fe–Ti increased to 18% and 24%, no large-scale hexagonal primary carbides can be seen (Figs. 2(d) and 2(e)). It indicates that the microstructure of the surfacing layer has changed from hypereutectic to eutectic and hypoeutectic.

Fig. 2.

The OM images of high chromium iron base hardfacing alloy with different Fe–Ti additions (a) 0 wt.% Fe–Ti, (b) 6 wt.% Fe–Ti, (c) 12 wt.% Fe–Ti, (d) 18 wt.% Fe–Ti, (e) 24 wt.% Fe–Ti. (Online version in color.)

The SEM images of high chromium iron base hardfacing alloy with different addition of titanium is shown in Fig. 3. the eutectic colonies which are composed of M₃(C, B) and austenite surrounds primary M₇(C, B)₃ carbides in the microstructure of Ti-free hardfacing alloy (Fig. 3(a)). In the solidification process, the primary M₇(C, B)₃ carbides are formed first from the high temperature molten pool. The addition of chromium, carbon and boron in the residual molten pool is reduced because the elements are consumed to form M₇(C, B)₃ carbides. Simultaneously, the austenite and eutectic M₃(C, B) carbides are precipitated around the large size primary M₇(C, B)₃ carbides. Therefore, the Ti-free hardfacing alloy exhibits a hypereutectic microstructure. When the Fe–Ti addition is 6 wt.%, the pipe shaped TiC is observed in the microstructure, and the size of primary M₇(C, B)₃ carbides are decreased (Fig. 3(b)). As the Fe–Ti addition further increased to 12%, the quantity of pipe shaped TiC is increased while the size of primary M₇(C, B)₃ carbides are further decreased (Fig. 3(c)). However, the hypereutectic microstructure changed to eutectic structure since the primary M₇(C, B)₃ carbides are disappeared for the hardfacing alloy with 18 wt.% Fe–Ti addition (Fig. 3(d)). The microstructure changes from the eutectic structure to the hypoeutectic one since the Fe–Ti addition reaches 24 wt.%. The change in microstructures is due to the formation of TiC which consumed carbon in the solidification process.

Fig. 3.

The SEM images of high chromium iron base hardfacing alloy with different Fe–Ti additions (a) 0 wt.% Fe–Ti, (b) 6 wt.% Fe–Ti, (c) 12 wt.% Fe–Ti, (d) 18 wt.% Fe–Ti, (e) 24 wt.% Fe–Ti.

Furthermore, Fig. 4 shows the EDS spectrum of matrix of Ti-free and ‐containing welding overlays. The results indicate that the degree of alloy of the matrix with chromium is increased with the increase of Fe–Ti addition. The addition of Fe–Ti increases the Cr content in the matrix, as Ti is prone to combine with C to from TiC and thus consumes a significant C content, resulting in considerably less formation of M₇(C, B)₃ carbides and higher dissociative Cr content in the molten pool, which forms solid solutions in the matrix in the following solidification process.

Fig. 4.

The EDS spectrum of matrix of Ti-free and ‐containing welding overlays (a) 0 wt.% Fe–Ti, (b) 24 wt.% Fe–Ti. (Online version in color.)

Figure 5 shows the polarization curve of welding overlays with different Fe–Ti additions in 3.5 wt.%NaCl solution + 0.01 mol/L HCl solution. With the increase of the amount of Fe–Ti in the welding wire, the polarization curve position of each welding overlay also shows the trend of first decreasing and then increasing. When the addition of Fe–Ti is 12%, it has the lowest self-corrosion potential and the largest self-corrosion current density.

Fig. 5.

Polarization curve of welding overlays with different Fe–Ti additions in 3.5 wt.%NaCl solution + 0.01 mol/L HCl solution. (Online version in color.)

Table 3 shows the polarization test results of samples with different Ti–Fe additions in 3.5 wt.%NaCl solution + 0.01 mol/L HCl solution. As the addition of Fe–Ti increasing from 6 wt.% to 12 wt.%, I_corr increases sharply from 5.97 × 10⁻⁶A/cm² to 401.02 × 10⁻⁶A/cm², and the corrosion resistance decreases dramatically. Figure 6 shows the trend chart of I_corr and E_corr of welding overlays with different Fe–Ti additions. E_corr is decreased firstly and then increased, in contract, I_corr is increased firstly and then decreased. The corrosion resistance of the welding overlay is the lowest when Fe–Ti addition is 12 wt.%, and the Ti-free overlay has the best corrosion resistance.

Table 3. The polarization test results of samples with different Fe–Ti additions in 3.5 wt.%NaCl solution +0.01 mol/L HCl solution.

Fe–Ti additions (wt.%)	Ecorr (V)	Icorr (10−6A/cm2)
0	−0.976	3.096
6	−0.978	5.97
12	−0.996	401.02
18	−0.985	8.063
24	−0.981	6.55

Fig. 6.

Trend chart of I_corr and E_corr of welding overlays with different Fe–Ti additions. (Online version in color.)

Figure 7 shows the Nyquist curve of welding overlays with different Fe–Ti additions in 3.5 wt.% NaCl solution + 0.01 mol/L HCl solution and the equivalent circuit. Z′ is the real impedance and Z" is the imaginary impedance, W is the Warburg impedance, R_s is the solution resistance, and R_ct is the charge transfer resistance. The R_ct is always used to evaluate the susceptibility to corrosion, and the higher R_ct value represents a lower corrosion current density and thus a better corrosion resistance.²⁸⁾ Figure 7(a) shows a compressed semicircular capacitive reactance arc. but there was a capacitive reactance arc in high frequency region and a straight line at a certain angle in low frequency region in 7(b). The straight line in the low frequency region reveals the existence of diffusion process known as Warburg impedance.²⁹⁾ The transformation of EIS curve is mainly attributed to the change of the kinetics of corrosion procedure, possibly from charge transfer control to diffusion control. The equivalent circuit element values are shown in Table 4. It can be seen from Fig. 8 that when the addition of Fe–Ti is increased from 0 wt.% to 12 wt.%, R_ct is decreased continuously. At Fe–Ti addition of 12 wt.%, the minimum value of R_ct is 6.857 × 10² Ω·cm², and the corrosion resistance of the welding overlay is the lowest. When the addition of Fe–Ti is increased from 12 wt.% to 24 wt.%, the value of R_ct is increased gradually, which indicates that the corrosion resistance of the alloy is increased again.

Fig. 7.

Nyquist curve of welding overlays with different Fe–Ti additions in 3.5 wt.% NaCl solution + 0.01 mol/L HCl solution. (Online version in color.)

Table 4. The values of the equivalent circuit elements for the impedance spectra measured in 3.5 wt.%NaCl solution + 0.01 mol/L HCl solution.

Fe–Ti additions (wt.%)	Equivalent circuit elements
	Rs (Ω·cm2)	Q (Ω·cm2)	Rct (Ω·cm2)	W (Ω·cm2)
0	2.618 × 104	6.604 × 10−11	6.265 × 105	–
6	1.921 × 104	1.170 × 10−10	4.439 × 105	–
12	1.980 × 102	9.372 × 10−6	6.857 × 102	5.995 × 10−3
18	2.475 × 104	7.640 × 10−6	5.264 × 105	–
24	1.674 × 104	3.533 × 10−11	8.439 × 105	–

Fig. 8.

Change trend of R_ct value with different Fe–Ti additions.

Figure 9 shows the microstructure of welding overlays with different Fe–Ti additions after acid corrosion by OM. The surface of large size primary M₇(C, B)₃ carbides and eutectic M₃ (C, B) carbides remains intact in the microstructure of Ti-free hardfacing alloy (Fig. 9(a)). When the addition of Fe–Ti is 6 wt.%, as shown in Fig. 9(b), the size of primary M₇(C, B)₃ carbides is decreased significantly, and a few quadrilateral TiC is formed. The different type of carbides are still intact after enduring acidic corrosion. Moreover, the network matrix structure around eutectic carbides is more refined, which is corroded seriously. The microstructure of the welding overlay is transformed into dense network eutectic structure when the addition of Fe–Ti is 12 wt.%. Due to the severe corrosion reaction, the corrosion degree of eutectic structure is increased significantly, and the depth of corrosion pit formed by corrosion of matrix part in eutectic structure is also increased (Fig. 9(c)). Combined with the analysis results of electrochemical test (Fig. 5), it can be proved that the corrosion resistance of the welding overlay is decreased with the increase of eutectic structure proportion, and the corrosion resistance is the lowest at Fe–Ti addition of 12 wt.%. With the further increased from 12 wt.% to 24 wt.%, the proportion of TiC structure is further increased, and the eutectic structure of surfacing layer is more refined. The corrosion occurs at the matrix structure since the microstructure of welding overlay is composed of TiC and fine network eutectic structure (Figs. 9(d) and 9(e)).

Fig. 9.

Microstructure of welding overlays with different Fe–Ti additions after acid corrosion by OM (a) 0 wt.% Fe–Ti, (b) 6 wt.% Fe–Ti, (c) 12 wt.% Fe–Ti, (d) 18 wt.% Fe–Ti, (e) 24 wt.% Fe–Ti. (Online version in color.)

Figure 10 shows the microstructure of welding overlays with different Fe–Ti additions after acid corrosion by SEM. When the addition of Fe–Ti is increased to 12 wt.%, the size of primary carbides is refined and the proportion of eutectic structure is increased. When the addition of ferrotitanium is 12 wt.%, the microstructure of the welding overlay is composed of eutectic structure, and the corrosion reaction of the alloy is the most severe. Further increasing of Fe–Ti addition increases the proportion of TiC and the Cr content in the matrix, thus increases the corrosion resistance of the welding overlay.

Fig. 10.

Microstructure of welding overlays with different Fe–Ti additions after acid corrosion by SEM (a) 0 wt.% Fe–Ti, (b) 6 wt.% Fe–Ti, (c) 12 wt.% Fe–Ti, (d) 18 wt.% Fe–Ti, (e) 24 wt.% Fe–Ti.

Figure 11 shows SEM mapping analysis of welding overlays with different Fe–Ti additions after corrosion. The results show that Cr and Ti are mainly distributed in the non-corroded area of the welding overlays. The corrosion mainly occurs in the matrix structure, and the surface of carbides including primary carbides, eutectic carbides and TiC remains intact. Cr is mainly concentrated in primary carbides and network eutectic carbides in the microstructure of Ti-free welding overlay. When the addition of Fe–Ti is increased from 0 wt.% to 6 wt.%, the TiC structure is formed (Figs. 11(a) and 11(b)). At the Fe–Ti addition of 12 wt.% (Fig. 11(c)), the distribution of Cr element is consistent with eutectic structure, which is in network or radial distribution. With the further increase of Fe–Ti addition, the welding overlay is gradually transformed into the composition of TiC and eutectic structure. Moreover, the distribution area of TiC structure is gradually expanded (Figs. 11(d) and 11(e)).

Fig. 11.

SEM mapping analysis of welding overlays with different Fe–Ti additions after corrosion (a) 0 wt.% Fe–Ti, (b) 6 wt.% Fe–Ti, (c) 12 wt.% Fe–Ti, (d) 18 wt.% Fe–Ti, (e) 24 wt.% Fe–Ti. (Online version in color.)

Due to the existence of potential difference between carbides and matrix, electric couple can be formed between different phases due to different potential. At this time, austenite matrix is used as anode and carbide as cathode due to its high self-corrosion potential. The electrode reaction of the welding overlays in 3.5 wt.% NaCl + 0.01 mol/l HCl solution is as follows:   

$$\mathrm{A}\mathrm{n}\mathrm{o}\mathrm{d}\mathrm{i}\mathrm{c}\mathrm{\hspace{0.17em} }\mathrm{r}\mathrm{e}\mathrm{a}\mathrm{c}\mathrm{t}\mathrm{i}\mathrm{o}\mathrm{n}:\mathrm{\hspace{0.17em} }\mathrm{\hspace{0.17em} }\mathrm{F}\mathrm{e}=\mathrm{F}{\mathrm{e}}^{2+}+2{\mathrm{e}}^{-}$$(1)

  

$$\mathrm{C}\mathrm{a}\mathrm{t}\mathrm{h}\mathrm{o}\mathrm{d}\mathrm{i}\mathrm{c}\mathrm{\hspace{0.17em} }\mathrm{r}\mathrm{e}\mathrm{a}\mathrm{c}\mathrm{t}\mathrm{i}\mathrm{o}\mathrm{n}:\mathrm{\hspace{0.17em} }\mathrm{\hspace{0.17em} }2{\mathrm{H}}^{+}+2{\mathrm{e}}^{-}={\mathrm{H}}_2\uparrow$$(2)

  

$$\mathrm{O}\mathrm{v}\mathrm{e}\mathrm{r}\mathrm{a}\mathrm{l}\mathrm{l}\mathrm{\hspace{0.17em} }\mathrm{r}\mathrm{e}\mathrm{a}\mathrm{c}\mathrm{t}\mathrm{i}\mathrm{o}\mathrm{n}:\mathrm{\hspace{0.17em} }\mathrm{\hspace{0.17em} }\mathrm{F}\mathrm{e}+2{\mathrm{e}}^{-}=\mathrm{F}{\mathrm{e}}^{2+}+{\mathrm{H}}_2$$(3)

The proportion of each phase in the microstructure plays an important role in the corrosion behavior of multiphase materials.³⁰⁾ Thus, the change of volume fraction of each phase in the welding overlays inevitably affects its corrosion resistance. Eutectic carbides can separate the matrix and have more boundaries than primary carbides. With the increase of Fe–Ti addition, the proportion of eutectic structure in the welding overlay is increased, and its corrosion resistance presents a decreasing trend firstly, which is caused by the increase of eutectic structure proportion and the refinement of primary M₇(C, B)₃ carbides. However, the corrosion resistance of the alloy increases with the increase of the volume fraction of TiC since the addition of Fe–Ti exceeds 18 wt.%.

4. Conclusions

In this study, the corrosion resistance of slag-free self-shielded flux-cored welding overlays with different Fe–Ti additions in 3.5 wt.% NaCl+0.01 mol/L HCl acidic solution was investigated. The main conclusions are as follows:

(1) The corrosion occurs in the matrix rather than M₇(C, B)₃, M₃(C, B) and TiC in the microstructure of all the slag-free self-shielded flux-cored welding overlays.

(2) The corrosion resistance of hypereutectic welding overlay is decreased when the Fe–Ti addition is increased from 0 wt.% to 12 wt.%.

(3) The corrosion resistance of the alloy is the lowest since the welding overlay is eutectic structure at the Fe–Ti addition of 12 wt.%. This is because the eutectic structure increases the interface of corrosion reaction, which accelerates the corrosion rate and increases the corrosion current in the electrochemical testing process.

(4) With the Fe–Ti addition increasing from 12 wt.% to 24 wt.%, the corrosion resistance of the welding overlays with hypoeutectic structure is gradually increased, owing to the increase of the proportion of TiC and chromium content in the matrix.

Acknowledgements

This work is supported by Anhui Provincial Natural Science Foundation (Grant No. 2208085ME135), China Postdoctoral Science Foundation Funded Project (Grant No. 2016M601753), Natural Science Foundation of Jiangsu Province (Grant No. BK20201453), Major Projects of Natural Science Research in Colleges and Universities in Jiangsu (Grant No. 19KJA460009), and Graduate Research and Innovation Projects of Jiangsu Province (Grant No. KYCX21_3450).

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