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Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature
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CERAMICS INTERNATIONAL
Ceramics International ] (]]]]) ]]]–]]] www.elsevier.com/locate/ceramint
Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature X. Shana,b, L.Q. Weia,n, P. Liuc, X.M. Zhanga, W.X. Tanga,b, P. Qiana, Y. Hea,b, S.F. Yea a
State Key Laboratory of Multiphase Complex Systems, Institute of Process Engineering, Chinese Academy of Sciences, PO Box 353, Beijing 100190, China b University of Chinese Academy of Sciences, No. 19(A) Yuquan Road, Beijing 100049, China c Shougang Research Institute of Technology, Beijing 100043, China Received 4 March 2014; accepted 14 April 2014
Abstract A CoO glass–ceramic was coated on 200 stainless steel and its thermal shock resistance and anti-oxidation effect were detected at 600–1250 1C in ambient air. This coating was prepared by a slurry method and it exhibited fairly good adhesion, oxidation resistance and stability at elevated temperature. Specifically, its thermal shock resistance and anti-oxidation effect were detected. The coating optimized was prepared by a slurry– thermal reaction. Metalloscope, SEM-EDX, and XRD revealed that a stable glass–ceramic layer was formed during the coating process which acted as a perfect film with the thermal cycles and prevented the 200 stainless steel from being oxidized. In the thermal cycle process, the glass– ceramic film was non-stripping with good CTE (coefficient of thermal expansion) match between coating and the steel. This low-cost and facile operating method can be used widely in stainless steel protection at high temperature. & 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Keywords: C. Thermal shock resistance; D. Glass–ceramic; CoO coating; Stainless steel; Oxidation resistance
1. Introduction Glass–ceramics are composite materials made by high temperature melting, forming, heat treatment combining with crystal and glass [1–4]. With high mechanical strength, adjustable thermal expansion property, excellent thermal shock resistance and chemical corrosion property and other superior performances, it is widely used in mechanical manufacture, optics, electronics and microelectronics, aerospace, chemical industry, biological medicine, etc [5–8]. Especially in machinery and chemical, glass– ceramic coatings are successfully applied in the material manufacturing and coating technology owing to its thermal properties. Achieving coatings or materials with thermal resistance is an important issue of industry hotspot [2,9]. Alone, in thermal power plants, the heating surface of boiler tubes is easy to be corroded due to the severe operating condition including chemical corrosion and intermittent operation (generally temperature range of n
Corresponding author. Tel.: þ86 10 82544899. E-mail address: [email protected] (L.Q. Wei).
20–1250 1C). Frequent change of boiler tubes brings about a large amount of wastes in steel and energy. So it is desirable to develop a thermal shock resistant protective coating with good adhesion and easy handling method. However, in industry, at present, crack grows amazingly in the coating during the cycling of hot–cold process, and the coating spalls at once due to the wide range of temperatures. Besides, internal or external surface oxidation (oxidants such as O2, H2O and SO2, in the furnace atmosphere) accelerates the cracking process [10,11]. Previous work done by our team such as the development of MgO coating series [12] were not thermal shock resistant which were in line with the requirements of iron and steel enterprise [12–14]. Adopting Sol–gel method [15–17] and other method such as Plasma Spraying [18,19] either require specific expensive devices or should be delivered in a rigid operation condition. By the way, high quality glass–ceramic technology is still a key technical challenge due to many factors [20–22]. Therefore, there is considerable motivation to improve the thermal shock resistance, in other words, to modify the adhesion between coating and steel, at the same time, slow
http://dx.doi.org/10.1016/j.ceramint.2014.04.078 0272-8842/& 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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down the high temperature oxidation process during the heating process. The most effective countermeasure is to develop a homogeneous coating by tailoring the composites [20,21]. Moreover, the low-cost slurry–thermal reaction makes it possible to develop an efficient glass–ceramic coating. Then, by selecting certain composition, it is possible to develop a proper coating to satisfy all the requirements above, but now little deep research was performed on its thermal-shock– oxidation resistance by the slurry–thermal reaction for stainless steel at high temperatures. With this aim in view, a CoO glass–ceramic coating in order to enhance its thermal shock resistance and oxidation resistance was prepared on the 200 stainless steel by adopting a cheap and convenient slurry–thermal reaction. The effects on thermal shock resistance and oxidation behavior of the steel at a range of 600– 1250 1C in air were discussed. In the end, a suggesting adhesion and oxidation resistant mechanism is stated. 2. Experimental 2.1. Coating preparation Table 1 shows the formula of the CoO coating used in this test. On the one hand, the composition of which was selected after a series of repeated tests. The raw materials were ballmilled with three times of the water (by weight) for about 10 h. On the other hand, all the coated samples were exposed to post-heat treatment by temperature-gradient method in a muffle furnace. The heating mechanism is as follows: First, the coated samples were heated to 200 1C in 30 min, then, within 40 min, the specimens were heated to 800 1C and after another 40 min, the temperature reached 1100 1C. Finally, they were preserved at 1100 1C for 30 min. 2.2. Steel surface preparation and coating application Industrial AISI 200 stainless steel was cut into specimen size of 50 50 3 mm plates by wire cutting machine and their chemical composition are shown in Table 2. The specimens were washed with alcohol and acetone in an ultrasonic bath in order to keep the surface clean. A dip-coating method was adopted to obtain a homogeneous film on the steel. The thickness of the coating was about 20–200 μm. Table 1 Chemical composition (wt%) of the glass coating.
2.3. Oxidation test and characterization methods The isothermal oxidation kinetic effect of the protective CoO coating aiming at reducing the oxidation rate was detected by thermogravimetric analysis device (PRKD-RD01) with a maximum range of 500 g, sensitivity of 70.01 mg and collecting data once per minute. The heating rate was about 7 1C/min up to 1100 1C, and when the temperature reached 1100 1C, the weight gains automatically measured by the device were continuously recorded for another 6 h. The composition and structure of glass–ceramic coating at the interface after heating at 1100 1C were characterized using field-emission scanning electron microscopy (SEM) via an electron microscope (JEOL 2100F, operating at 15 kV), equipped with an energy dispersive X-ray detector. X-ray diffraction (XRD, PANalytical B.V., the Netherlands) patterns of the coating were measured on a Panalytical X’Pert PRO system using Cu-Kα radiation in the diffraction angle (2θ) range 51–901. Crystalline phase was identified by the Jade 5.0 software to refer the related peaks to the standard diffraction in database (JCPDS). 2.4. Evaluation of thermal shock resistance Thermal shock test was performed to evaluate the resistance of coating for frequent changes in temperature [23] and to examine whether the CoO coating obtained could withstand harsh thermal changes. The coated specimens were subjected to thermal cycling by placing them into muffle furnaces maintained at 600 and 700 1C for 5 min and subsequently cooled down in air (Beijing winter at average 5 1C) for another 5 min till the temperature reaches down to below 100 1C in the atmospheric conditions. The maximum thermal cycling times of 600 and 700 was counted and the thermal cycling process was repeated until coating failed. Meanwhile, the textures of the coated specimens, especially the fracture centers (containing a certain amount of Fe), were characterized by Metallographic Microscope (Olympus BX51M) and the numbers of the fracture centers after a dynamic tracking of 5 times, 10 times, 15 times reheating were counted until obvious patches of fracture appeared. 3. Results and discussion 3.1. Effect of glass–ceramic coating
SiO2
Al2O3
ZnO
BaO
B2O3
CaO
CoO
MoO3
42
3
4
24
3.5
4
18
1.5
3.1.1. CoO coating morphology The glass–ceramic CoO coating powder melted at 800– 900 1C based on a series of coating sintering experiments at
Table 2 Chemical composition (wt%) of 200 stainless steel sample. C
Cr
Ni
Fe
P
Si
Mn
N
S
0.12–0.25
16.5–18.0
1–1.75
Balance
r0.060
r1.0
14.0–15.0
0.32–0.40
r 0.03
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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500–1200 1C both on the stainless steel substrates and empty alundum crucibles every 100 1C, when the molting conditions of the coating powders at different temperatures were observed. Direct sintering of the coating on stainless steel at 1200 1C or higher led to the formation of different microstructures such as dendritic and irregular triangle-spherular morphology, as is displayed in Fig. 1(a) and Fig. 1(b). This kind of coating is an inhomogeneous layer adhered firmly on the steel substrate. Meanwhile, the experiments operated at 800 1C or lower temperatures showed that functional elements did not work or form a dense film. When heated after soaking at 1100 1C for 30 min, there were two different phases formed in the coating, as shown in Fig. 1(c) and Fig. 1(d). XRD results reveal that the CoO coating is composed of anorthite, while the uncoated sample is Fe2O3 phase after reheated at 1100 1C for 30 min. 3.1.2. Oxidation test Two sets of experiments were carried out during the oxidation tests. First, weight gain experiments have been done and the weight gains versus heating times for the bare and coated 200 stainless steel after isothermal period at 1100 1C for 9 h are shown in Fig. 3, in which the weight gains of the coated specimen is much lower than that of the bare sample. As shown in Fig. 2(a), XRD data indicates that the bare specimen
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has been oxidized and the main oxide is Fe2O3. On the contrary, the coated sample is covered by a well-proportioned glass–ceramic coating which consists of anorthite. Second, the oxidation loss has been evaluated over time after 3, 6, 9 h oxidation at a constant 1100 1C, 1150 1C and 1250 1C in a muffle furnace in stagnant air, and after the process, the bare specimens and the coated ones were taken out and then cooled down in ambient air ( 10 1C). Then the coated specimens were polished carefully on a SiC polishing paper of 1200 mesh to remove the dense coating as the adhesion between the steel substrate and the coating is too firm to remove by water quenching. All of the samples were weighted before and after oxidation (the scales of the bare samples were removed by external mechanical force such as hammer and pinchers), the oxidation losses under different temperatures were calculated and shown in Fig. 4. From it, it's quite obvious that the steel loss rate reduces significantly after coated and as a block to protect the steel substrate from being oxidized, the glass–ceramic coating plays an important role. However, the bare samples were severely oxidized by the atmosphere in the muffle furnace and the surface of the steel was large uneven with sparse irregular channels. Then the coated specimen was embedded by resin, polished on a SiC polishing pad of 200, 800, 1200 and finally 2000 mesh in order to be prepared for cross-sectional observation by SEM, the images of which are shown in Fig. 5. The glass–ceramic
Fig. 1. (a) SEM image ( 5000) of the CoO coating after crystallization at 1200 1C. (b) SEM image ( 20,000) of the CoO coating after crystallization at 1250 1C. (c) The morphology under metalloscope ( 200) of the CoO coating after formation at 1100 1C. (d) The morphology under metalloscope ( 500) of the CoO coating after formation at 1100 1C. Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Fig. 2. (a) XRD pattern of the uncoated sample. (b) XRD pattern of the coated sample. The former is coated with CoO, the latter is coated without CoO.
coating was a dense film with an average thickness of 20–200 μm. As is shown in Fig. 5, a Si-rich layer can be obviously seen by EDS elemental mapping and in this layer there is less Fe than other places. 3.1.3. Thermal cycling test The supreme advantage of glass–ceramics is that they produce excellent thermochemical properties because they are impervious to thermal shock [20–22]. The coated specimens were in comparison to the bare ones on thermal cycling and the maximum thermal cycling at 600 and 700 1C were counted until the observation of any corrosion points as are
shown in Fig. 6. With temperature changes of 600 and 700 1C, constant thermal shock exposes the substrate and forms ferric oxide, which can be demonstrated by EDS in Fig. 7. So in the thermal cycling test, the number of the corrosion points was counted in a dynamic feedback process to evaluate the thermal shock resistance of the CoO coating and any observation of corrosion points was treated as the failure of the coating. It is known that with the rise in temperature, the thermal shock resistance of the coating decrease rapidly. For instance, when heated to 600 1C, the coating had suffered from 25 times of thermal shock cycling, however, when heated to 700 1C, the coating only could only withstand 20 times of cycling before
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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the formation of any single corrosion point. By counting the numbers of the corrosion points after every 5 times under Metalloscope on the geometric center of the substrate, a
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dynamic tracing was conducted and shown in Fig. 8. From which, it is easy to draw the conclusion that the CoO coating could endure more than 20 times thermal cycling. It is worth noting that when corrosion points appeared, the coating still did not crack until more than 80 times (at 600 1C) of thermal cycling compared with that of 60 times at (900 1C). 3.2. Protection mechanism
Fig. 3. Oxidation weight changes of coated and bare sample of the 200 stainless steel at isothermal 1100 1C.
3.2.1. Mechanism of coating enhancing oxidation resistance of the stainless steel At elevated temperature, all the samples follow the parabolic law [12,14,28] and the increasing oxidation is attributed to poor adhesion between scale and substrate, segregation of SiO2 at scale interface and scale spallation resulting from interfacial defects and thermal stresses [24]. According to the oxidation mechanism, the enhancement of the oxidation resistance of the 200 stainless steel by CoO glass–ceramic coating may base on the following explanation. Ultimately, it is a matter of controlling inward diffusion of oxygen. On the one hand, the formation of a dense,
Fig. 4. Oxidation losses of 200 stainless steel specimens after oxidation at differernt temperatures in ambient air: (a) at 1100 1C; (b) at 1150 1C; (c) at 1250 1C; (d) oxidation loss of the coated specimens at different temperatures. Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Fig. 5. EDS mapping of the cross-sectional microstructures of the coated sample.
well-adherent CoO coating works to protect the stainless steel substrate from being oxidized. In other words, the scale and the substrate tightly bond so as to block the oxygen from inward diffusion, which decreases the oxidation rate. The outward diffusion of Cr ions from the stainless steel to the inside scale is the primary step, which results in the formation of Cr2O3 [14,25,26]. As can be seen in the EDS lines in Fig. 9, at about 12.5 μm, it is obvious that there is formation of Cr2O3, which serves as an excellent barrier of diffusion, such as the inward O and outward Fe, etc [14]. As is shown in Fig. 2(b), the former represents the XRD pattern of the coating with CoO and the latter shows the one without CoO. However, peaks appear at almost the same angle. From Fig. 2(b), it is clear that the structure of anorthite formed in the coating, after putting a certain amount of CoO into the slurry and sintering, the original structure was doped by Co2 þ [21,27], and decreased the degree of crystallization. After mechanical removals of the scales on the coated CoO specimen and the one without CoO, both of the samples expose metallic substrates, which indicates that the formation of the doped structure and the original anorthite help to block the inward diffusion of oxygen. Furthermore, the formation of doping structure reduces the thermal stress [21]. On the other hand, Si element plays the role to prevent stainless steel substrate from being oxidized. The source of Si
includes inward Si from the coating and the outward Si from the stainless steel. The diffusion of Si can be traced by EDS mapping of the cross section of coated specimen, as are presented in Fig. 9. From Fig. 9, it's certain that a Si-rich layer exists in the bonding section of the coated specimen. Meanwhile, EDS line scans for Si also shows the phenomenon of a Si-rich layer, which can be obviously seen in Fig. 5 and the outward diffusion of Si from the steel reacted with oxygen and formed the Si-rich layer [12,25]. The formation of the layer serves as a supreme barrier to decrease the inward diffusion of oxygen. So the well oxidation resistance is attributed to the synergistic effect of the outside formation of Co2 þ doped anorthite, middle Cr2O3 layer and the inside Si-rich layer. 3.2.2. Mechanism of coating enhancing thermal shock resistance Single Cr2O3 film, due to its CTE mismatch with steel which gives rise to the thermal stresses, is easy to crack and spall when the temperature suddenly drops [29,30]. Scale delamination is the result of CTE mismatch [21]. First, The Co2 þ doping modifies the CTE of anorthite (4.82 10 6/1C) (Ayhan Mergen, 2003), matching for 200 series stainless steel. Then, Shaigan et al. [24] argue that the function element of Si serves to prevent scale from being
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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spalled. As is shown in Fig. 5, the Si-rich layer works to bond with the coating and substrate. At the same time, the formations of amorphous phase Ba–Si–B–O and crystalline phase have excellent thermal shock resistance [20,21]. In
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contrast to temporary protection, the CoO coating serves as a long-term protection. The failure mechanism of the coating is followed by the generation of corrosion points, then, the development of crack, the extension of flaws [31,32], and finally the joint of the cracks, as was traced by the dynamic thermal cycling test. 4. Conclusions A glass–ceramic CoO coating designed for durable protective application was successfully prepared on the 200 stainless steel by slurry–thermal reaction conveniently and economically. The obtained coating would function at 1100 1C and higher, transforming into a homogeneous, dense, and glass– ceramic coating. Thermal shock test performed at 600–900 1C
Fig. 6. The morphology of the coated samples before (a) and after (b) 25 times thermal cycling.
Fig. 8. The number of corrosion points after thermal cycling at different temperature.
Fig. 7. The EDS element diffusion shows the corrosion point is mainly made up of Fe2O3. Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Fig. 9. EDS line scanning of the cross-section of the coated sample shows the existence of Cr2O3.
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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in muffle furnace showed that, the glass–ceramic CoO coating endured more than 50 times of thermal cycling and at the same time, steel loss reduced to nearly zero, which greatly expands the usage of stainless steel in a variety of temperature range. This study indicates that this CoO coating can be an applicable choice to protect stainless steel in stainless steel industry. Acknowledgements This work was strongly supported by Natural Science Foundation of China (No. 51202249), the 863 Project (2011AA06A104), and Projects in the National Science & Technology Pillar Program during the 12th Five-year Plan Period (2011BAC06B01, 2012BAB08B04). The authors thank all the members in the Material Chemistry and Engineering Group, the State Key Lab. of Multiphase Complex Systems, Chinese Academy of Sciences. References [1] W. Höland, G.H. Beall, Glass–Ceramic Technology, second ed., Wiley, Hoboken, 2012. [2] E.D. Zanotto, A bright future for glass–ceramics, Am. Ceram. Soc. Bull. 89 (2010) 20. [3] R.K. Chinnam, A.A. Francis, J. Will, E. Bernardo, A.R. Boccaccini, Review. Functional glasses and glass–ceramics derived from iron rich waste and combination of industrial residues, J. Non-Cryst. Solids 365 (2013) 63. [4] A. Theocharopoulos, X. Chen, R. Hill, M.J. Cattell, Reduced wear of enamel with novel fine and nano-scale leucite glass–ceramics, J. Dent. 41 (2013) 562. [5] J.A. Juhasz, S.M. Best, Bioactive ceramics: processing, structures and properties, J. Mater. Sci. 47 (2012) 612. [6] T. Kokubo, M. Shigematsu, Y. Nagashima, M. Tashiro, T. Nakamura, T. Yamamuro, S. Higashi, Apatite-and wollastonite-containing glass– ceramics for prosthetic application, Bull. Inst. Chem. Res. 60 (1982) 260. [7] T. Komatsu, T. Honma, Optical active nano-glass–ceramics, Int. J. Appl. Glass Sci. 4 (2013) 125. [8] M. Tatsumisago, A. Hayashi, Nanoscale Technology for Advanced Lithium Batteries, Springer, New York, 2014, p. 65–66. [9] I. Denry, J.A. Holloway, Low temperature sintering of fluorapatite glass– ceramics, Dent. Mater. 30 (2014) 112. [10] J.W. Evans, The evolution of technology for light metals over the last 50 years: Al, Mg, And Li, JOM 59 (2007) 37. [11] I.M. Morsi, H.H. Ali, Kinetics and mechanism of silicothermic reduction process of calcined dolomite in magnetherm reactor, Int. J. Miner. Process. (2014), http://dx.doi.org/10.1016/j.minpro.2013.11.016. [12] X. Zhou, S.F. Ye, H.W. Xu, P. Liu, X.J. Wang, L.Q. Wei, Influence of ceramic coating of MgO on oxidation behavior and descaling ability of low alloy steel, Surf. Coat. Technol. 206 (2012) 3620. [13] L.Q. Wei, P. Liu, S.F. Ye, Preparation and properties of anti-oxidation inorganic nano-coating for low carbon steel at an elevated temperature, J. Wuhan Univ. Technol. 21 (2006) 49.
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Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature X. Shana,b, L.Q. Weia,n, P. Liuc, X.M. Zhanga, W.X. Tanga,b, P. Qiana, Y. Hea,b, S.F. Yea a
State Key Laboratory of Multiphase Complex Systems, Institute of Process Engineering, Chinese Academy of Sciences, PO Box 353, Beijing 100190, China b University of Chinese Academy of Sciences, No. 19(A) Yuquan Road, Beijing 100049, China c Shougang Research Institute of Technology, Beijing 100043, China Received 4 March 2014; accepted 14 April 2014
Abstract A CoO glass–ceramic was coated on 200 stainless steel and its thermal shock resistance and anti-oxidation effect were detected at 600–1250 1C in ambient air. This coating was prepared by a slurry method and it exhibited fairly good adhesion, oxidation resistance and stability at elevated temperature. Specifically, its thermal shock resistance and anti-oxidation effect were detected. The coating optimized was prepared by a slurry– thermal reaction. Metalloscope, SEM-EDX, and XRD revealed that a stable glass–ceramic layer was formed during the coating process which acted as a perfect film with the thermal cycles and prevented the 200 stainless steel from being oxidized. In the thermal cycle process, the glass– ceramic film was non-stripping with good CTE (coefficient of thermal expansion) match between coating and the steel. This low-cost and facile operating method can be used widely in stainless steel protection at high temperature. & 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Keywords: C. Thermal shock resistance; D. Glass–ceramic; CoO coating; Stainless steel; Oxidation resistance
1. Introduction Glass–ceramics are composite materials made by high temperature melting, forming, heat treatment combining with crystal and glass [1–4]. With high mechanical strength, adjustable thermal expansion property, excellent thermal shock resistance and chemical corrosion property and other superior performances, it is widely used in mechanical manufacture, optics, electronics and microelectronics, aerospace, chemical industry, biological medicine, etc [5–8]. Especially in machinery and chemical, glass– ceramic coatings are successfully applied in the material manufacturing and coating technology owing to its thermal properties. Achieving coatings or materials with thermal resistance is an important issue of industry hotspot [2,9]. Alone, in thermal power plants, the heating surface of boiler tubes is easy to be corroded due to the severe operating condition including chemical corrosion and intermittent operation (generally temperature range of n
Corresponding author. Tel.: þ86 10 82544899. E-mail address: [email protected] (L.Q. Wei).
20–1250 1C). Frequent change of boiler tubes brings about a large amount of wastes in steel and energy. So it is desirable to develop a thermal shock resistant protective coating with good adhesion and easy handling method. However, in industry, at present, crack grows amazingly in the coating during the cycling of hot–cold process, and the coating spalls at once due to the wide range of temperatures. Besides, internal or external surface oxidation (oxidants such as O2, H2O and SO2, in the furnace atmosphere) accelerates the cracking process [10,11]. Previous work done by our team such as the development of MgO coating series [12] were not thermal shock resistant which were in line with the requirements of iron and steel enterprise [12–14]. Adopting Sol–gel method [15–17] and other method such as Plasma Spraying [18,19] either require specific expensive devices or should be delivered in a rigid operation condition. By the way, high quality glass–ceramic technology is still a key technical challenge due to many factors [20–22]. Therefore, there is considerable motivation to improve the thermal shock resistance, in other words, to modify the adhesion between coating and steel, at the same time, slow
http://dx.doi.org/10.1016/j.ceramint.2014.04.078 0272-8842/& 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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down the high temperature oxidation process during the heating process. The most effective countermeasure is to develop a homogeneous coating by tailoring the composites [20,21]. Moreover, the low-cost slurry–thermal reaction makes it possible to develop an efficient glass–ceramic coating. Then, by selecting certain composition, it is possible to develop a proper coating to satisfy all the requirements above, but now little deep research was performed on its thermal-shock– oxidation resistance by the slurry–thermal reaction for stainless steel at high temperatures. With this aim in view, a CoO glass–ceramic coating in order to enhance its thermal shock resistance and oxidation resistance was prepared on the 200 stainless steel by adopting a cheap and convenient slurry–thermal reaction. The effects on thermal shock resistance and oxidation behavior of the steel at a range of 600– 1250 1C in air were discussed. In the end, a suggesting adhesion and oxidation resistant mechanism is stated. 2. Experimental 2.1. Coating preparation Table 1 shows the formula of the CoO coating used in this test. On the one hand, the composition of which was selected after a series of repeated tests. The raw materials were ballmilled with three times of the water (by weight) for about 10 h. On the other hand, all the coated samples were exposed to post-heat treatment by temperature-gradient method in a muffle furnace. The heating mechanism is as follows: First, the coated samples were heated to 200 1C in 30 min, then, within 40 min, the specimens were heated to 800 1C and after another 40 min, the temperature reached 1100 1C. Finally, they were preserved at 1100 1C for 30 min. 2.2. Steel surface preparation and coating application Industrial AISI 200 stainless steel was cut into specimen size of 50 50 3 mm plates by wire cutting machine and their chemical composition are shown in Table 2. The specimens were washed with alcohol and acetone in an ultrasonic bath in order to keep the surface clean. A dip-coating method was adopted to obtain a homogeneous film on the steel. The thickness of the coating was about 20–200 μm. Table 1 Chemical composition (wt%) of the glass coating.
2.3. Oxidation test and characterization methods The isothermal oxidation kinetic effect of the protective CoO coating aiming at reducing the oxidation rate was detected by thermogravimetric analysis device (PRKD-RD01) with a maximum range of 500 g, sensitivity of 70.01 mg and collecting data once per minute. The heating rate was about 7 1C/min up to 1100 1C, and when the temperature reached 1100 1C, the weight gains automatically measured by the device were continuously recorded for another 6 h. The composition and structure of glass–ceramic coating at the interface after heating at 1100 1C were characterized using field-emission scanning electron microscopy (SEM) via an electron microscope (JEOL 2100F, operating at 15 kV), equipped with an energy dispersive X-ray detector. X-ray diffraction (XRD, PANalytical B.V., the Netherlands) patterns of the coating were measured on a Panalytical X’Pert PRO system using Cu-Kα radiation in the diffraction angle (2θ) range 51–901. Crystalline phase was identified by the Jade 5.0 software to refer the related peaks to the standard diffraction in database (JCPDS). 2.4. Evaluation of thermal shock resistance Thermal shock test was performed to evaluate the resistance of coating for frequent changes in temperature [23] and to examine whether the CoO coating obtained could withstand harsh thermal changes. The coated specimens were subjected to thermal cycling by placing them into muffle furnaces maintained at 600 and 700 1C for 5 min and subsequently cooled down in air (Beijing winter at average 5 1C) for another 5 min till the temperature reaches down to below 100 1C in the atmospheric conditions. The maximum thermal cycling times of 600 and 700 was counted and the thermal cycling process was repeated until coating failed. Meanwhile, the textures of the coated specimens, especially the fracture centers (containing a certain amount of Fe), were characterized by Metallographic Microscope (Olympus BX51M) and the numbers of the fracture centers after a dynamic tracking of 5 times, 10 times, 15 times reheating were counted until obvious patches of fracture appeared. 3. Results and discussion 3.1. Effect of glass–ceramic coating
SiO2
Al2O3
ZnO
BaO
B2O3
CaO
CoO
MoO3
42
3
4
24
3.5
4
18
1.5
3.1.1. CoO coating morphology The glass–ceramic CoO coating powder melted at 800– 900 1C based on a series of coating sintering experiments at
Table 2 Chemical composition (wt%) of 200 stainless steel sample. C
Cr
Ni
Fe
P
Si
Mn
N
S
0.12–0.25
16.5–18.0
1–1.75
Balance
r0.060
r1.0
14.0–15.0
0.32–0.40
r 0.03
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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500–1200 1C both on the stainless steel substrates and empty alundum crucibles every 100 1C, when the molting conditions of the coating powders at different temperatures were observed. Direct sintering of the coating on stainless steel at 1200 1C or higher led to the formation of different microstructures such as dendritic and irregular triangle-spherular morphology, as is displayed in Fig. 1(a) and Fig. 1(b). This kind of coating is an inhomogeneous layer adhered firmly on the steel substrate. Meanwhile, the experiments operated at 800 1C or lower temperatures showed that functional elements did not work or form a dense film. When heated after soaking at 1100 1C for 30 min, there were two different phases formed in the coating, as shown in Fig. 1(c) and Fig. 1(d). XRD results reveal that the CoO coating is composed of anorthite, while the uncoated sample is Fe2O3 phase after reheated at 1100 1C for 30 min. 3.1.2. Oxidation test Two sets of experiments were carried out during the oxidation tests. First, weight gain experiments have been done and the weight gains versus heating times for the bare and coated 200 stainless steel after isothermal period at 1100 1C for 9 h are shown in Fig. 3, in which the weight gains of the coated specimen is much lower than that of the bare sample. As shown in Fig. 2(a), XRD data indicates that the bare specimen
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has been oxidized and the main oxide is Fe2O3. On the contrary, the coated sample is covered by a well-proportioned glass–ceramic coating which consists of anorthite. Second, the oxidation loss has been evaluated over time after 3, 6, 9 h oxidation at a constant 1100 1C, 1150 1C and 1250 1C in a muffle furnace in stagnant air, and after the process, the bare specimens and the coated ones were taken out and then cooled down in ambient air ( 10 1C). Then the coated specimens were polished carefully on a SiC polishing paper of 1200 mesh to remove the dense coating as the adhesion between the steel substrate and the coating is too firm to remove by water quenching. All of the samples were weighted before and after oxidation (the scales of the bare samples were removed by external mechanical force such as hammer and pinchers), the oxidation losses under different temperatures were calculated and shown in Fig. 4. From it, it's quite obvious that the steel loss rate reduces significantly after coated and as a block to protect the steel substrate from being oxidized, the glass–ceramic coating plays an important role. However, the bare samples were severely oxidized by the atmosphere in the muffle furnace and the surface of the steel was large uneven with sparse irregular channels. Then the coated specimen was embedded by resin, polished on a SiC polishing pad of 200, 800, 1200 and finally 2000 mesh in order to be prepared for cross-sectional observation by SEM, the images of which are shown in Fig. 5. The glass–ceramic
Fig. 1. (a) SEM image ( 5000) of the CoO coating after crystallization at 1200 1C. (b) SEM image ( 20,000) of the CoO coating after crystallization at 1250 1C. (c) The morphology under metalloscope ( 200) of the CoO coating after formation at 1100 1C. (d) The morphology under metalloscope ( 500) of the CoO coating after formation at 1100 1C. Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Fig. 2. (a) XRD pattern of the uncoated sample. (b) XRD pattern of the coated sample. The former is coated with CoO, the latter is coated without CoO.
coating was a dense film with an average thickness of 20–200 μm. As is shown in Fig. 5, a Si-rich layer can be obviously seen by EDS elemental mapping and in this layer there is less Fe than other places. 3.1.3. Thermal cycling test The supreme advantage of glass–ceramics is that they produce excellent thermochemical properties because they are impervious to thermal shock [20–22]. The coated specimens were in comparison to the bare ones on thermal cycling and the maximum thermal cycling at 600 and 700 1C were counted until the observation of any corrosion points as are
shown in Fig. 6. With temperature changes of 600 and 700 1C, constant thermal shock exposes the substrate and forms ferric oxide, which can be demonstrated by EDS in Fig. 7. So in the thermal cycling test, the number of the corrosion points was counted in a dynamic feedback process to evaluate the thermal shock resistance of the CoO coating and any observation of corrosion points was treated as the failure of the coating. It is known that with the rise in temperature, the thermal shock resistance of the coating decrease rapidly. For instance, when heated to 600 1C, the coating had suffered from 25 times of thermal shock cycling, however, when heated to 700 1C, the coating only could only withstand 20 times of cycling before
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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the formation of any single corrosion point. By counting the numbers of the corrosion points after every 5 times under Metalloscope on the geometric center of the substrate, a
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dynamic tracing was conducted and shown in Fig. 8. From which, it is easy to draw the conclusion that the CoO coating could endure more than 20 times thermal cycling. It is worth noting that when corrosion points appeared, the coating still did not crack until more than 80 times (at 600 1C) of thermal cycling compared with that of 60 times at (900 1C). 3.2. Protection mechanism
Fig. 3. Oxidation weight changes of coated and bare sample of the 200 stainless steel at isothermal 1100 1C.
3.2.1. Mechanism of coating enhancing oxidation resistance of the stainless steel At elevated temperature, all the samples follow the parabolic law [12,14,28] and the increasing oxidation is attributed to poor adhesion between scale and substrate, segregation of SiO2 at scale interface and scale spallation resulting from interfacial defects and thermal stresses [24]. According to the oxidation mechanism, the enhancement of the oxidation resistance of the 200 stainless steel by CoO glass–ceramic coating may base on the following explanation. Ultimately, it is a matter of controlling inward diffusion of oxygen. On the one hand, the formation of a dense,
Fig. 4. Oxidation losses of 200 stainless steel specimens after oxidation at differernt temperatures in ambient air: (a) at 1100 1C; (b) at 1150 1C; (c) at 1250 1C; (d) oxidation loss of the coated specimens at different temperatures. Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Fig. 5. EDS mapping of the cross-sectional microstructures of the coated sample.
well-adherent CoO coating works to protect the stainless steel substrate from being oxidized. In other words, the scale and the substrate tightly bond so as to block the oxygen from inward diffusion, which decreases the oxidation rate. The outward diffusion of Cr ions from the stainless steel to the inside scale is the primary step, which results in the formation of Cr2O3 [14,25,26]. As can be seen in the EDS lines in Fig. 9, at about 12.5 μm, it is obvious that there is formation of Cr2O3, which serves as an excellent barrier of diffusion, such as the inward O and outward Fe, etc [14]. As is shown in Fig. 2(b), the former represents the XRD pattern of the coating with CoO and the latter shows the one without CoO. However, peaks appear at almost the same angle. From Fig. 2(b), it is clear that the structure of anorthite formed in the coating, after putting a certain amount of CoO into the slurry and sintering, the original structure was doped by Co2 þ [21,27], and decreased the degree of crystallization. After mechanical removals of the scales on the coated CoO specimen and the one without CoO, both of the samples expose metallic substrates, which indicates that the formation of the doped structure and the original anorthite help to block the inward diffusion of oxygen. Furthermore, the formation of doping structure reduces the thermal stress [21]. On the other hand, Si element plays the role to prevent stainless steel substrate from being oxidized. The source of Si
includes inward Si from the coating and the outward Si from the stainless steel. The diffusion of Si can be traced by EDS mapping of the cross section of coated specimen, as are presented in Fig. 9. From Fig. 9, it's certain that a Si-rich layer exists in the bonding section of the coated specimen. Meanwhile, EDS line scans for Si also shows the phenomenon of a Si-rich layer, which can be obviously seen in Fig. 5 and the outward diffusion of Si from the steel reacted with oxygen and formed the Si-rich layer [12,25]. The formation of the layer serves as a supreme barrier to decrease the inward diffusion of oxygen. So the well oxidation resistance is attributed to the synergistic effect of the outside formation of Co2 þ doped anorthite, middle Cr2O3 layer and the inside Si-rich layer. 3.2.2. Mechanism of coating enhancing thermal shock resistance Single Cr2O3 film, due to its CTE mismatch with steel which gives rise to the thermal stresses, is easy to crack and spall when the temperature suddenly drops [29,30]. Scale delamination is the result of CTE mismatch [21]. First, The Co2 þ doping modifies the CTE of anorthite (4.82 10 6/1C) (Ayhan Mergen, 2003), matching for 200 series stainless steel. Then, Shaigan et al. [24] argue that the function element of Si serves to prevent scale from being
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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spalled. As is shown in Fig. 5, the Si-rich layer works to bond with the coating and substrate. At the same time, the formations of amorphous phase Ba–Si–B–O and crystalline phase have excellent thermal shock resistance [20,21]. In
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contrast to temporary protection, the CoO coating serves as a long-term protection. The failure mechanism of the coating is followed by the generation of corrosion points, then, the development of crack, the extension of flaws [31,32], and finally the joint of the cracks, as was traced by the dynamic thermal cycling test. 4. Conclusions A glass–ceramic CoO coating designed for durable protective application was successfully prepared on the 200 stainless steel by slurry–thermal reaction conveniently and economically. The obtained coating would function at 1100 1C and higher, transforming into a homogeneous, dense, and glass– ceramic coating. Thermal shock test performed at 600–900 1C
Fig. 6. The morphology of the coated samples before (a) and after (b) 25 times thermal cycling.
Fig. 8. The number of corrosion points after thermal cycling at different temperature.
Fig. 7. The EDS element diffusion shows the corrosion point is mainly made up of Fe2O3. Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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Fig. 9. EDS line scanning of the cross-section of the coated sample shows the existence of Cr2O3.
Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078
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in muffle furnace showed that, the glass–ceramic CoO coating endured more than 50 times of thermal cycling and at the same time, steel loss reduced to nearly zero, which greatly expands the usage of stainless steel in a variety of temperature range. This study indicates that this CoO coating can be an applicable choice to protect stainless steel in stainless steel industry. Acknowledgements This work was strongly supported by Natural Science Foundation of China (No. 51202249), the 863 Project (2011AA06A104), and Projects in the National Science & Technology Pillar Program during the 12th Five-year Plan Period (2011BAC06B01, 2012BAB08B04). The authors thank all the members in the Material Chemistry and Engineering Group, the State Key Lab. of Multiphase Complex Systems, Chinese Academy of Sciences. References [1] W. Höland, G.H. Beall, Glass–Ceramic Technology, second ed., Wiley, Hoboken, 2012. [2] E.D. Zanotto, A bright future for glass–ceramics, Am. Ceram. Soc. Bull. 89 (2010) 20. [3] R.K. Chinnam, A.A. Francis, J. Will, E. Bernardo, A.R. Boccaccini, Review. Functional glasses and glass–ceramics derived from iron rich waste and combination of industrial residues, J. Non-Cryst. Solids 365 (2013) 63. [4] A. Theocharopoulos, X. Chen, R. Hill, M.J. Cattell, Reduced wear of enamel with novel fine and nano-scale leucite glass–ceramics, J. Dent. 41 (2013) 562. [5] J.A. Juhasz, S.M. Best, Bioactive ceramics: processing, structures and properties, J. Mater. Sci. 47 (2012) 612. [6] T. Kokubo, M. Shigematsu, Y. Nagashima, M. Tashiro, T. Nakamura, T. Yamamuro, S. Higashi, Apatite-and wollastonite-containing glass– ceramics for prosthetic application, Bull. Inst. Chem. Res. 60 (1982) 260. [7] T. Komatsu, T. Honma, Optical active nano-glass–ceramics, Int. J. Appl. Glass Sci. 4 (2013) 125. [8] M. Tatsumisago, A. Hayashi, Nanoscale Technology for Advanced Lithium Batteries, Springer, New York, 2014, p. 65–66. [9] I. Denry, J.A. Holloway, Low temperature sintering of fluorapatite glass– ceramics, Dent. Mater. 30 (2014) 112. [10] J.W. Evans, The evolution of technology for light metals over the last 50 years: Al, Mg, And Li, JOM 59 (2007) 37. [11] I.M. Morsi, H.H. Ali, Kinetics and mechanism of silicothermic reduction process of calcined dolomite in magnetherm reactor, Int. J. Miner. Process. (2014), http://dx.doi.org/10.1016/j.minpro.2013.11.016. [12] X. Zhou, S.F. Ye, H.W. Xu, P. Liu, X.J. Wang, L.Q. Wei, Influence of ceramic coating of MgO on oxidation behavior and descaling ability of low alloy steel, Surf. Coat. Technol. 206 (2012) 3620. [13] L.Q. Wei, P. Liu, S.F. Ye, Preparation and properties of anti-oxidation inorganic nano-coating for low carbon steel at an elevated temperature, J. Wuhan Univ. Technol. 21 (2006) 49.
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Please cite this article as: X. Shan, et al., Influence of CoO glass–ceramic coating on the anti-oxidation behavior and thermal shock resistance of 200 stainless steel at elevated temperature, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.04.078