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Microstructural characteristics and protection performances of plasma-sprayed Al2O3–Al composite coatings on AZ91D magnesium alloy

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Science and Engineering of Composite Materials
From the journal Science and Engineering of Composite Materials Volume 23 Issue 5

Abstract

Four Al2O3-Al composite coatings were successfully fabricated on AZ91D alloy by plasma sprayed with changing ratios of Al2O3 and Al mixed powders, respectively. XRD results indicate that all the composite coatings are composed of γ-Al2O3, α-Al2O3, and Al. SEM and EDS analysis find that Al2O3-Al composite coatings present the interlaced structures of Al and Al2O3 bands. VIDAS image analysis reveals that the porosities of the composite coatings are increased by adding Al2O3. In the composite coatings, the hardness of Al is about 62 HV and that of Al2O3 is up to 1380 HV. The electrochemical polarization tests testify that Al2O3-Al composite coatings can effectively protect AZ91D alloy from corroding in a chloride environment. The wear test results confirm that the wear resistance of Al2O3-Al composite coatings is markedly superior to that of AZ91D alloy. The excellent protection degrees are attributed to their particular compositions, microstructures, and properties. Moreover, the effect of Al2O3 contents on the microstructures and protection performances of Al2O3-Al composite coatings was also studied and discussed in detail.

Keywords: composite coating; corrosion resistance; microstructural characteristic; plasma spraying; wear resistance

1 Introduction

Magnesium alloys have been widely used in the automotive, aerospace, and electronic industries for their unique properties, such as low density, high specific strength and excellent mechanical castability [1, 2]. Unfortunately, magnesium alloys are highly susceptible to corrosion, especially in environments containing aggressive ions as chloride ions, sulfate ions, etc. Moreover, they are soft and have low wear resistance [3, 4]. These shortages are greatly restricting their wider applications. One of the most effective ways to prevent corrosion and abrasion is to fabricate adequate protection coating. All the time researches on suitable coating materials and corresponding preparation methods become the focus by researchers, who are engaged in protection works for magnesium alloys [5].

Al2O3 ceramic coating deposited on metallic substrates by plasma spraying have received considerable attention for good corrosion resistance and good wear resistance [6–8]. However, the single Al2O3 coating presents porous layer microstructures and poor intersplat bonding, which is determined by the characteristic of plasma spraying [9, 10]. Especially, it is often obtained lower bond strength between Al2O3 ceramic and the metallic substrate due to their biggest difference of thermal expansion coefficient, which to a great extent impedes regular services of plasma-sprayed Al2O3 ceramic coating on effective protection, particularly under some harsh operating conditions.

Some existing researches have shown that the ceramic metal composite material by incorporating a second metallic phase into ceramic matrices can successfully improve mechanical properties and obtain higher bond strength [11, 12]. Al, being an excellent ductility and thermal conductivity of material, is a good candidate added to prepare Al2O3-Al composite material for plasma spraying. By plasma spraying, Al2O3-Al composite coatings have been successfully deposited on different substrates, such as stainless steel, magnesium alloy and polymer [13–15]. These studies reveal that the composite coating possesses improve microstructure, mechanical properties and bond strength with the substrates. Moreover, it has been testified that plasma-sprayed Al2O3-Al composite coatings largely enhance the corrosion resistance and wear resistance of the substrate materials.

This paper aimed to study and analyze the anticorrosion and antiwear protection degree of plasma-sprayed Al2O3-Al composite coating for AZ91D substrate. At the same time, the effects of Al2O3 contents on the microstructures and protection performances of the composite coatings were studied and discussed in detail.

2 Materials and methods

Commercial extruded AZ91D magnesium alloy was used as substrate for plasma spraying. The substrate was ground with abrasive paper up to 1000 grit, cleaned with acetone, and then sandblasted using 40–60 mesh corundum before plasma spraying. Commercially pure Al and α-Al2O3 powders were used as the feedstock materials. The particle size and shape were confirmed by scanning electron microscope, as shown in Figure 1. The size of pure Al powders was range of 50–200 μm, and that of Al2O3 powders was 10–50 μm. The mixed powders of Al and Al2O3 were deposited on the substrate by atmosphere plasma spraying equipment (Praxair3710, Danbury, CT, USA) to fabricate four Al2O3-Al composite coatings on AZ91D alloy. In four composite coatings, the volume percentages of Al2O3 are 22.4%, 35.6%, 50.0%, 67.0%, respectively. Then, these coatings with the increasing of Al2O3 were orderly designated as composite coating A, composite coating B, composite coating C, and composite coating D. For comparison, pure Al coating also was prepared on AZ91D. In this work, the same plasma spraying parameters were applied to produce all the coatings, as given in Table 1. The thickness of all sprayed coatings was about 250–300 μm.

Figure 1 SEM images of as-received feedstock Al and Al2O3 powders in the experiments (A) pure Al powders (B) Al2O3 powders.
Figure 1

SEM images of as-received feedstock Al and Al2O3 powders in the experiments (A) pure Al powders (B) Al2O3 powders.

Table 1

Plasma spraying parameters for pure Al and Al2O3-Al mixed powders.

ParametersValue
Arc current/A700
Arc voltage/V50
Primary gas (Ar)/MPa0.41
Secondary gas (H2)/MPa0.21
Carrier gas (Ar)/MPa0.17
Spraying distance/mm100

The microstructures of Al2O3-Al composite coatings and pure Al coating were observed by S-3400 N scanning electron microscope (SEM) attached EDS. VIDAS image analysis system was adopted to examine the porosities of the coatings. The phase structures of all the coatings were identified by RIGAKU ULTIMA4 diffractometer (XRD) with Cu Kα radiation, voltage 40 KV, and current 40 mA. The electrochemical corrosion resistance of the composite coatings and pure Al coating was measured in 3.5 wt% NaCl solution by using an Ivium electrochemical system. The work electrodes were the coating samples. Pt electrode and saturated calomel electrode (SCE) were used as the counter and the reference electrode, respectively. Before the measurement, all the coating samples were immersed in NaCl solution for 30 min to reach a steady open circuit potential. Then, polarization scan was started at a scanning rate of 0.1 mV/s. Vickers microhardness was evaluated at the polished cross section of as-sprayed coatings using a FM-300 microhardness tester under the load of 50 N with a dwell time of 5 s. Dry sliding friction and wear tests were performed in a pin-on-disc mode on a wear testing machine (MWW-1A) at 20 N, one sliding velocity of 2.3 m/min, and 10 min test duration. Number 240 sandpaper was selected as the counterpart. The weight loss was measured by using an electronic balance with a precision scale of 0.0001 g. To ensure the reproducibility of the measurements, three tests were conducted under the same test conditions for AZ91D substrate and each composite coating sample.

3 Results and discussion

3.1 Phase analysis

X-ray diffraction (XRD) was performed for determining the compositions and the relative amount of the phases in the plasma-sprayed coatings. Figure 2A shows XRD patterns of pure Al coating, and the phase is only Al as naturally expected. Figure 2B shows XRD patterns of Al2O3-Al composite coatings. It is obvious that the composite coatings are composed of γ-Al2O3, α-Al2O3, and Al. According to XRD results, it can be concluded that α-Al2O3 in the starting powders mostly converted into γ-Al2O3 after spraying. It is attributed that γ-Al2O3 tends to be nucleated from the melt in preference to α-Al2O3 at the high cooling rate due to relatively lower interfacial energy between crystal and liquid [16]. Moreover, it is obvious that the Al2O3 peaks ascend and Al peaks descend with the increase of Al2O3 ratios in the composite coatings.

Figure 2 XRD diffraction patterns of (A) pure Al coating, (B) Al2O3-Al composite coatings.
Figure 2

XRD diffraction patterns of (A) pure Al coating, (B) Al2O3-Al composite coatings.

3.2 Microstructure characteristics

Figure 3A shows the microstructure morphologies of plasma-sprayed pure Al coating. In Al coating, no splat structure is found, which indicates that Al powders have completely melted during plasma spraying. Molten Al droplets quickly impact the as-sprayed surface. The metallurgical reaction can occur between the latter Al splats with high temperature and the former Al splats, and the result is that the compacted structure is formed. Figure 3B–E shows the microstructures of plasma-sprayed Al2O3-Al composite coating A–D on AZ91D substrate, respectively. It can be seen that all the Al2O3-Al composite coatings present the gray and white interlaced microstructures. EDS analysis indicates that the chemical compositions of gray bands are Al, and these of white bands are Al and O, as shown in Figure 3F. Combined with the previous XRD results, it can be confirmed that the gray structure are Al and white structure are Al2O3. The Al structures in the composite coatings are also dense, and white Al2O3 structures are evidently increasing from composite coating A to composite coating D. Figure 4 gives the interface morphologies of pure Al coating and Al2O3-Al composite coatings. It can be seen that the interface of Al phase and magnesium alloy is not obvious for all the coating samples, which is attributed the good interface combination between them due to occur metallurgical reaction of Al and magnesium alloys [14]. It also can be found that more and more Al2O3 structure distributes in the interface regions with adding Al2O3 in the composite coatings, which will affect on the interface combination of the coating and substrate. In addition, some obvious pores can be observed in the composite coatings, which are related with the characteristics of plasma-spray coatings. Moreover, the pores in these Al2O3-Al composite coatings mainly formed in Al2O3 structures. VIDAS analysis results show that the porosity of pure Al coating is only 0.6%, which is corresponding to its dense microstructure. The porosities of the Al2O3-Al composite coatings are increased with increasing Al2O3 in the coatings. The porosities of the composite coating A, B, C, and D are 1.4%, 2.5%, 8.3%, and 22.4%, respectively. However, it is worth mentioning that these pores are not continuous from the outmost surface of the coating down to AZ91D substrate.

Figure 3 SEM morphologies and compositions of as-sprayed pure Al coating and Al2O3-Al composite coatings (A) pure Al coating; (B–E) composite coating A, B, C, and D, (F) EDS spectra.
Figure 3

SEM morphologies and compositions of as-sprayed pure Al coating and Al2O3-Al composite coatings (A) pure Al coating; (B–E) composite coating A, B, C, and D, (F) EDS spectra.

Figure 4 The interface morphologies of (A) pure Al coating and (B–E) Al2O3-Al composite coating A-D.
Figure 4

The interface morphologies of (A) pure Al coating and (B–E) Al2O3-Al composite coating A-D.

In order to study in detail the microstructure characteristics of sprayed Al and Al2O3-Al composite coatings, all the coatings were carefully observed in a greater magnification. The results were that three especial morphologies were found, as presented in Figure 5. The first special morphology is that there are a few of beads both in pure Al coating and in the composite coatings, as shown in Figure 5A. The second is that tiny Al2O3 splats can be observed from a magnified Al2O3 band in the composite coatings, and there are some obvious pores between the Al2O3 splats, as shown in Figure 5B. The third is that there are a spot of unshaped particles in the composite coatings, as shown in Figure 5C. According to their shapes and EDS analysis, it can be concluded that these particles are partially melted Al2O3.

Figure 5 Higher magnification view of Al2O3-Al composite coatings.
Figure 5

Higher magnification view of Al2O3-Al composite coatings.

It is well known that the plasma-sprayed microstructure is mainly related to the feedstock melting state, which is determined by the temperature distributions of the inflight particle [17]. During plasma spraying, the temperature of as-sprayed Al powders and Al2O3 powders is increased when they pass through the jet due to the heating effect from the plasma flame. Under normal circumstances, all the powders are fully melted because of the high temperature caused by plasma flame. When the sprayed droplets impact on the rough surface at higher velocities, splashing will occur [18]. Al powders with low melting points are completely melted, molten Al droplets impact on the sprayed surface and take place splashing. The global splash produces, that is Al beads, are formed and retained in the composite coating. From Figure 5A, it can be observed that the size of Al beads is significantly smaller than that of the initial Al particles. Comparing to Al, the Al2O3 powders have higher melting point. Although they also are completely melted after heating by plasma flame, the latter Al2O3 plats with high temperature cannot highly fuse with the former Al2O3 plats. Simultaneously, some pores are formed between Al2O3 plats. The result is that the tiny splat structures with some pores are observed on Al2O3 bands, as shown in Figure 5B.

However, it must be mentioned that the heating states of feedstock are also affected by different flight trajectories [19]. During plasma spraying, it is inevitable that a spot of sprayed powders, especially Al2O3 particles with high melting points, will fly off the central heating. They may only be partially melted and retained in the coatings after impacting on the substrate, as observed in Figure 5C.

3.3 Corrosion performance

Figure 6 presents the typical potentiodynamic polarization curves for pure Al coating and Al2O3-Al composite coatings in a 3.5 wt% NaCl solution. For comparison, the polarization curve for AZ91D substrate is also given in Figure 6. The AZ91D substrate has the lowest corrosion potential (about -1.44V), and its corrosion current density is the highest up to 4.40 A/cm2. On the contrary, the pure Al coating presents the highest corrosion potential (about -1.29 V) and the lowest corrosion current density (approximately 1.87×10-2 A/cm2). Simultaneously, it can be obviously observed that all the Al2O3-Al composite coatings have higher corrosion potentials and lower corrosion current densities than AZ91D substrate. The results indicate that Al2O3-Al composite coatings have better corrosion protection for AZ91D. However, their protection degrees are still lower than that of sprayed pure Al coating.

Figure 6 Potentiodynamic polarization curves for AZ91D substrate, pure Al coating, and Al2O3-Al composite coatings.
Figure 6

Potentiodynamic polarization curves for AZ91D substrate, pure Al coating, and Al2O3-Al composite coatings.

The corrosion resistance of the coating mainly is attributed to its chemical compositions and microstructures. It is known that both Al2O3 and Al in Al2O3-Al composite coatings have good corrosion resistance, and no new phases formed at the interface between Al2O3 and Al during plasma spraying, which is testified by the previous XRD results. Moreover, Al2O3 has no conductibility. So it is impossible to take place the galvanic reaction between Al2O3 and Al in corrosion intermediate. Furthermore, none of the pores is continuous from the outmost surface of the composite coating down to the AZ91D substrate. This is an important feature, suggesting that the coatings are impermeable to corrosive intermediate. So Al2O3-Al composite coating can act as an effective barrier between the corrosive intermediate and substrate and effectively eliminate the corrosion behavior of AZ91D alloy.

By further comparing the polarization curves of four Al2O3-Al composite coatings, it also can be concluded that the difference of Al2O3 contents has an obvious effect on the corrosion resistance of the Al2O3-Al composite coatings. For the composite coatings A and B, including relatively smaller Al2O3, their corrosion potential and corrosion density is the same level, which illuminates that the differences of their corrosion protection are very slight. When the volume of Al2O3 is added to the correspondence with that of Al, the composite coating C presents highest corrosion potential and lowest corrosion density. When the volume of Al2O3 is increased to exceed that of Al, such as composite coating D, comparing with composite coating C its corrosion potential decreases and corrosion density increases. This means that the corrosion protection degree of composite coating D decreases. In addition, the passive regions are observed for the composite coating C and composite coating D with more Al2O3, and a relatively large difference value of Epit-Ecorr (about 0.75 V) was found, indicating that the pitting of the two composite coatings has been greatly delayed. The passive behavior also was found in Spencer’s research work [20]. The variations of corrosion resistance of the composite coatings with adding Al2O3 should be related to the complex microstructural characteristics of Al2O3-Al composite coatings, such as different Al2O3 content, different porosity, and so on. On the whole, the composite coating C can provide the excellent corrosion protection degree for AZ91D substrate.

3.4 Microhardness and tribological properties

It is difficult to measure the bulk hardness of the Al2O3-Al composite coatings due to the thinner of the composite coatings (250–300 μm) and the special Al and Al2O3 interlaced microstructures. So the microhardness of Al and Al2O3 were tested in this work, respectively. For both structures, the measurement series comprise 10 indentations. The results show that in Al2O3-Al composite coatings the microhardness of Al is about 62 HV, and that of Al2O3 is approximate to 1380 HV. But it must point out that the bulk hardness of the composite coatings also will be enhanced with the increasing of hard Al2O3.

The friction coefficients are plotted versus wear time for AZ91D and four Al2O3 composite coatings, as shown in Figure 7A. The friction curves show that the composite coatings exhibit the same behaviors. At the initial stage, the curves are fluctuant and unsteady. After 2 min, the friction coefficients become relatively flat. Finally, the friction coefficient of composite coating A fluctuates between roughly 0.585 and 0.620. That of composite coating B is between 0.530 and 0.575. The friction coefficient of composite coating C remains between 0.310 and 0.355, and that of composite coating D changes from 0.345 to 0.420. It is obvious that the friction coefficients of all Al2O3-Al composite coating are lower than that of AZ91D alloy (between 0.640 and 0.715). Moreover, the composite coating C presents the lowest friction coefficient. Figure 7B shows the wear loss of AZ91D substrate and Al2O3-Al composite coatings against 240 SiC sand paper at room temperature. The weight loss of AZ91D is about 8.500×10-4 g/mm2, and those of composite A, B, C, and D are 4.006×10-4 g/mm2, 2.977×10-4 g/mm2, 1.812×10-4 g/mm2, and 0.880×10-4 g/mm2, respectively. It also can be found that the wear losses of the composite coatings are lower that that of AZ91D alloy, and the weight loss is decreased with increasing of Al2O3 in the coatings. These results fully show that the composite coatings effectively improve the wear resistance of magnesium alloy. It is generally accepted that the wear properties of plasma-sprayed coatings depends on the microstructure and thermal–mechanical properties [21]. According to previous structure analysis, it has known that the Al2O3-Al composite coating presents the morphology characteristics that the Al2O3 band distributes in Al matrix. During the wear testing, hard Al2O3 band presents good antiwear effect, and soft Al makes roles as good support and buffer. Additional, Al with good thermal conductivity in the composite coating is in favor for alleviating the concentration of the tribological heat and thermal stress on the real contact area of friction pairs [22].

Figure 7 Friction coefficient (A) and wear loss (B) of AZ91D and Al2O3-Al composite coatings.
Figure 7

Friction coefficient (A) and wear loss (B) of AZ91D and Al2O3-Al composite coatings.

Simultaneously, it can be confirmed that the effect of Al2O3 content on the tribological properties of Al2O3-Al composite coatings is also obvious, according to aforementioned friction coefficient curves and wear loss results. When the volume of Al2O3 is less than that of Al for composite coating A, B, and C, the bulk hardness of the composite coatings is increased with adding Al2O3, and the wear resistance of the coatings is gradually enhanced. So the friction coefficient and wear loss of the composite coatings are both decreasing with increasing Al2O3 structure. When the volume of Al2O3 is more than that of Al, such as composite coating D, the friction coefficient has a little increase instead. It may be relate with the relatively more porosity. The porosity usually acts to degrade the wear resistance of coatings [23]. Moreover, it must mention that the marginal coating of the composite coating D samples occurs to flake off during wearing. The possible reason is that the interface combination becomes worse due to its more Al2O3 at interface region, as shown in Figure 4. Another reason is ascribed that the toughness of composite coating with more hard Al2O3 is decreasing, which induces to brittle fracture in the margin of the composite coating. Although wear loss of composite coating D is the lowest, it is not a perfect Al2O3-Al composite coating for magnesium protection.

Synthetically considering all test results, it has been decided that the Al2O3-Al composite coating C will be attractively studied on the surface protection applications of AZ91D magnesium alloy in the further work due to its higher corrosion resistance and much excellent wear resistance.

4 Conclusions

Plasma-sprayed Al2O3-Al composite coatings were prepared by using different ratios of Al2O3 and Al mixed powders. Microstructural characteristics and protection properties of Al2O3-Al composite coatings were studied. The following points were found:

  1. The plasma-sprayed Al2O3-Al composite coatings are composed of γ-Al2O3, α-Al2O3, and Al. The composite coating presents interlaced structure of Al and Al2O3 bands. Al bonds present the denser structures, and Al2O3 bands show the splat structures with some pores. In addition, a few of Al beads and partial melted Al2O3 particles are retained in the composite coatings.

  2. The Al2O3-Al composite coating can offer sufficient corrosion protection for AZ91D substrate, which is related with its special microstructures and compositions. However, the protection degrees of the composite coatings are lower than that of sprayed pure Al coating. The Al2O3 contents in the coatings have an obvious effect on the polarization behavior of the composite coatings.

  3. In the composite coatings, the hardness of Al is about 62 HV, and that of Al2O3 is up to 1380 HV. The wear resistance of Al2O3-Al composite coatings is markedly higher than that of AZ91D substrate. The improvement in antiwear property of the composite coating can be attributed to the microstructure and thermal–mechanical properties of Al2O3-Al composite coatings. When the volume of Al2O3 is less than that of Al, the wear resistance of the composite coatings is enhanced with increasing Al2O3. When the volume of Al2O3 is higher than that of Al, the marginal of the composite coating occurs to flake off during wearing.

Corresponding author: Huanhuan Sun, School of Materials Science and Engineering, Shenyang Ligong University, No. 6, Nanping Center Road, Hunnan New District, Shenyang 110159, China, e-mail:

Acknowledgments

The work was supported by Science and Technology Research Project of the Education Department of Liaoning Province (L2012066).

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Received: 2014-5-23
Accepted: 2014-10-19
Published Online: 2015-1-20
Published in Print: 2016-9-1

©2016 Walter de Gruyter GmbH, Berlin/Boston

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Articles in the same Issue

  1. Frontmatter
  2. Original articles
  3. Microstructural characteristics and protection performances of plasma-sprayed Al2O3–Al composite coatings on AZ91D magnesium alloy
  4. Effects of poly(styrene-co-maleic anhydride) on the performance of LGF/TPU/ABS composites
  5. Influence of ultrasonic cavitation on microstructure and mechanical response of an aluminum/alumina nanocomposite
  6. Feasibility studies of cellulose microfiber (CMF) reinforced poly(ethylene-co-vinyl acetate) (EVA) composites for food packaging applications
  7. Laser surface treatment of aluminum composite: surface characteristics
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  10. Cooling rate effects on the crystallization kinetics of polypropylene/date palm fiber composite materials
  11. Microstructural, nanomechanical and wear properties of magnetic pulse electrodeposited Ni-TiN composite coatings
  12. Effect of cutting tool lead angle on machining forces and surface finish of CFRP laminates
  13. Identification of delamination defects through covariance of energy change: numerical modeling
  14. A study on the printability properties of alkali-sized recycled papers
  15. Preparation and microstructure of machinable Al2O3/mica composite by ball milling and hot-press sintering
https://doi.org/10.1515/secm-2014-0151
Keywords for this article
composite coating; corrosion resistance; microstructural characteristic; plasma spraying; wear resistance
Creative Commons
BY-NC-ND 3.0

Articles in the same Issue

  1. Frontmatter
  2. Original articles
  3. Microstructural characteristics and protection performances of plasma-sprayed Al2O3–Al composite coatings on AZ91D magnesium alloy
  4. Effects of poly(styrene-co-maleic anhydride) on the performance of LGF/TPU/ABS composites
  5. Influence of ultrasonic cavitation on microstructure and mechanical response of an aluminum/alumina nanocomposite
  6. Feasibility studies of cellulose microfiber (CMF) reinforced poly(ethylene-co-vinyl acetate) (EVA) composites for food packaging applications
  7. Laser surface treatment of aluminum composite: surface characteristics
  8. Non-isothermal crystallization behavior of polypropylene/zinc oxide composites
  9. Compression tests on square, thin-walled steel tube/bamboo-plywood composite hollow columns
  10. Cooling rate effects on the crystallization kinetics of polypropylene/date palm fiber composite materials
  11. Microstructural, nanomechanical and wear properties of magnetic pulse electrodeposited Ni-TiN composite coatings
  12. Effect of cutting tool lead angle on machining forces and surface finish of CFRP laminates
  13. Identification of delamination defects through covariance of energy change: numerical modeling
  14. A study on the printability properties of alkali-sized recycled papers
  15. Preparation and microstructure of machinable Al2O3/mica composite by ball milling and hot-press sintering
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