Durability and stability of superhydrophobic stainless steel mesh

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Materials and Interfaces

Durability and stability of superhydrophobic stainless steel mesh supported pure-silica zeolite beta coatings Yun Li, Xiufeng Liu, and Baoquan Zhang Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.9b00046 • Publication Date (Web): 24 Apr 2019 Downloaded from http://pubs.acs.org on April 24, 2019

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Industrial & Engineering Chemistry Research

Durability and stability of superhydrophobic stainless steel mesh supported pure-silica zeolite beta coatings

Yun Li, Xiufeng Liu, Baoquan Zhang*

State Key Laboratory of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300350, China

ABSTRACT: The poor durability and stability of superhydrophobic materials under various working conditions limit their widespread applications. Zeolite films have attracted considerable attention owing to their good mechanical, thermal and chemical stabilities. Stainless steel mesh (SSM) supported pure-silica zeolite beta (PSZB) coatings with superhydrophobicity have been fabricated using secondary growth method. The durability

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and stability of SSM-supported PSZB coatings were investigated thoroughly after undergone various treatments, including abrasion, corrosion, high-temperature and ultrasonication.

The

SSM-supported

PSZB

coatings

could

maintain

their

superhydrophobicity and high separation efficiencies above 99% with trace amount of oil contents in water as well as stable chloroform fluxes after abrasion for 80 cycles or exposure to corrosive media. The PSZB coating could keep a close attachment on the SSM support in high-temperature and ultrasonication environments. This work demonstrated the satisfactory durability and stability of SSM-supported PSZB coatings, and would give promise for zeolite-coated SSMs in actual oil/water separation.

1. INTRODUCTION Superwettable materials have been widely used in the field of oil/water separation1,2, unidirectional liquid penetration3 and other smart applications4,5. Of reported superwettable materials, stainless steel mesh (SSM) based materials with superhydrophobicity have drawn much attention to oil/water separation owing to their


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satisfactory performances and ease of operation.6 Polymers and inorganic substances have been employed to modify SSMs by spraying7,8, thermal polymerization9, combustion10, vacuum suction11, stacking12 and hydrothermal crystallization13. Although these materials exhibit high separation performances for a variety of oil/water mixtures, most of them would lose their superhydrophobicity when immersed in corrosive media, exposed to high-temperature environments or suffering mechanical damages as a result of the destruction of micro/nano-scale hierarchical structures and/or low-energy surface, eventually hindering development of their actual applications.14 Zeolites show excellent mechanical, thermal and chemical stabilities due to their dense crystalline backbone.15–17 Thus, it is desirable to fabricate robust zeolite films with special wetting ability for actual oil/water separation. Currently, there are only a few reports about SSM supported zeolite coatings with superwettability. Yu et al. designed the silicalite-1 coated SSM with superhydrophilicity and underwater superoleophobicity to separate water from oil.18 Kim et al. prepared the MFI-type zeolite-coated SSM using in situ crystallization method and studied the effect of Al/Si ratio on the membrane surface wettability.19 Guo et al. fabricated the silicalite-1 film on SSM with both


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superamphiphilicity in air and superoleophobicity underwater.20 In our previous work, the SSM-supported pure-silica zeolite beta (PSZB) coating was prepared by using the seeded-growth method.21 The rough hierarchical structure on the outer surface of synthesized SSM-supported PSZB coatings together with intrinsic hydrophobicity of PSZB give them with both superhydrophobicity and superoleophilicity. It was demonstrated that the SSM-supported PSZB coating exhibited high separation efficiencies for oil/water mixtures.21 However, the durability and stability of these materials have not been checked systematically on condition that they are exposed to rigorous operation conditions including high-temperature, strong corrosive media and mechanical damages. With respect to superhydrophobic SSM-supported PSZB coatings, the changes in both surface morphology and separation performances are going to be evaluated by way of abrasion, corrosion, heating and sonication in this contribution. It will be demonstrated that the SSM-supported PSZB coatings possess satisfactory mechanical durability, corrosion resistance and thermal stability. They could retain superhydrophobic characteristics and high separation performances after various treatments.


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2. EXPERIMENTAL SECTION 2.1. Synthesis of SSM-Supported PSZB Coatings. The detailed descriptions about materials and chemical reagents used in this experiment were available in Supporting Information. The SSM-supported PSZB coating was prepared by secondary growth method as reported previously.21 Firstly, the polydopamine modified method was employed to prepare seed layers on the surface of SSMs with high coverage degree. The dealuminated zeolite beta seeds were redispersed into freshly prepared Tris(hydroxy-methyl) aminomethane (Tris) buffer solution to form a 0.5 wt% suspension. The pre-prepared SSM (350 mesh, 3 × 3 cm) was immersed into the seed suspension with dopamine (DA) for 20 h, and dried at 60 °C. Then, the seeded SSM was treated in a synthesis gel with a molar composition of tetraethylammonium hydroxide (TEAOH) : SiO2 : hydrofluoric acid (HF) : H2O : n-propanol = 0.6 : 1.0 : 0.6 : 7 : 2.4. The fumed silica was dissolved in TEAOH solution at 80 °C under vigorously stirring. HF was added to the obtained synthesis gel, resulting in the formation of light yellow solid. Then to the above solid, n-propanol was added with stirring, forming a homogeneous gel. After aged for 24 h, the resultant gel was transferred to a Teflon-lined autoclave, where


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the seeded substrate was placed vertically. The hydrothermal treatment was carried out at 140 °C for 7 d. The as-synthesized samples were cleaned by deionized water (DI H2O), and dried with nitrogen (N2) purging. 2.2. Post-Synthetic Treatments. The abrasion on the SSM-supported PSZB coating was performed to investigate its mechanical durability. As shown in Figure 1, a sample was moved 10 cm on a piece of sandpaper (2000 mesh) at a speed of 5 cm s-1 under a load weighing of 25 g for a number of repeated cycles.22 To investigate the chemical stability of the PSZB coating, samples were subjected to corrosion in 0.1 M HCl, 0.1 M NaOH and 1 M NaCl for 24 h. After immersion, the samples were washed with DI H2O and ethanol, and then flushed with N2. The high-temperature treatment was carried out to demonstrate the thermal stability of SSM-supported PSZB coatings. The sample was heated to a set temperature and kept there for 1 h, and made the sample cool down at last. The ultrasonication treatment was employed to check the adhesive strength of the superhydrophobic coating on the support. Samples were subjected to sonication with 200 W in chloroform solvent for a specific time period. The samples after ultrasonication treatment were washed by ethanol and flushed with N2. The surface wettability of all


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treated samples was estimated according to the static water contact angle (WCA) measurement. The oil/water separation of treated SSM-supported PSZB coatings was also carried out to illustrate the effect of various treatments on separation performances.

Figure 1. The abrasion treatment of the SSM-supported PSZB coating on sandpaper. 2.3. Characterization. The morphologies of SSM-supported PSZB coatings were obtained on scanning electron microscopy (SEM, Hitachi S-4800). The surface wettability of SSM-supported PSZB coatings was measured by static WCAs (Dataphysics OCAH 200) with the drop size of ~ 3 μL. The final value was reported as the mean of three experiments. 2.4. Oil/Water Separation. The oil/water separation was conducted as reported previously.21 Chloroform permeated through the SSM-supported PSZB coating, while water was intercepted. The separation efficiency was defined according to % = (m1/m0)×100, for which m0 is the mass of water before the separation process and m1


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the mass of water intercepted in the upper tube.10 The residual oil content in water was measured by using a Ke-Chuang 9800 gas chromatograph equipped with a thermal conductivity detector. In addition, the chloroform flux was measured to describe the separation performance of the SSM-supported PSZB coatings.21 The setup was the same as the above separation system. Chloroform was poured, and the liquid level was maintained at the height of 10 cm. The volume (V) of permeated chloroform was recorded. The flux (F) was calculated according to F = V/(S×t), where S is the film area and t the permeation time.21 The final result was taken from three repeated experiments.

3. RESULTS AND DISCUSSION For actual applications, it is vital that superhydrophobic materials could maintain its micro/nano-scale hierarchical structure and low-energy surface under severe conditions. The mechanical durability of the SSM-supported PSZB coating was investigated via abrasion, which was carried out under a load weighing 25 g with sandpaper for multiple cycles. The variations of WCAs and chloroform/water separation


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efficiencies with abrasion cycles was displayed in Figure 2a. The untreated SSMsupported PSZB coating exhibited superhydrophobic characteristics with a WCA of 150.4 and a high separation efficiency of 99.6%. Compared with the pristine sample, it could be seen that WCAs had a slight fluctuation and were still greater than 150 even after 60 abrasion cycles. Once more than 80 abrasion cycles were carried out, the WCA decreased to approximately 148.9, suggesting a reduction in the superhydrophobicity of the SSM-supported PSZB coating. Despites the decreased WCA, the chloroform/water separation efficiency remained above 99% over 80 abrasion cycles. In addition, the measured residual oil content in water and chloroform flux were almost unchanged (Figure 2b). These results demonstrated that the SSM-supported PSZB coating had a superior mechanical durability under the abrasion treatment up to 80 cycles, which could be ascribed to the dense crystalline backbone of zeolite beta crystals.23 SEM images were displayed to illustrate the change of surface morphology after abrasion test (Figure 3). Figure 3a,b,g showed the morphology of untreated SSMsupported PSZB coatings. The intergrown PSZB crystal layer around 11 μm in thickness was fabricated on the SSM support to form a micro/nano-scale hierarchical


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structure with low surface energy. Figure 3c–f showed the corresponding surface structure of the SSM-supported PSZB coating after abrasion treatment under a load weighing 25 g for 20, 40, 60, and 80 times. The severe destruction on the surface was not observed and the intergrown truncated bipyramidal morphology remained over 60 abrasion cycles compared with the pristine sample. With the increase of abrasion cycles, the surface of the PSZB coating became smoother, indicating that the rough hierarchical structure was gradually destroyed. Although mild destruction was observed on the regions positioned at the top of the PSZB coating after 80 abrasion cycles, the nano-scale structure at its low position was well retained (Figure 3f). Furthermore, the cross-sectional view of the SSM-supported PSZB coating after 80 abrasion cycles was given in Figure 3h. Compared with the as-synthesized samples, the top layer after 80 abrasion cycles was smoother and exhibited a reduced thickness of ca. 9 μm. These observations were in accordance with the changes of WCAs and separation performances after abrasion treatments, further demonstrating the good mechanical durability of SSM-supported PSZB coatings.


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Figure 2. Variations of WCAs and chloroform/water separation efficiencies (a), and chloroform fluxes and residual oil contents in water (b) with abrasion cycles for SSMsupported PSZB coatings.


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Figure 3. SEM images of SSM-supported PSZB coatings: (a,b) as-synthesized samples; and (c–f) the samples after being abrased for 20, 40, 60, and 80 cycles. Cross-sectional views of SSM-supported PSZB coatings: (g) as-synthesized samples; and (h) the samples after being abrased for 80 cycles.


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To further evaluate the robustness of fabricated SSM-supported PSZB coatings, the corrosion treatment was performed by immersing them in corrosive media. The WCAs and chloroform/water separation efficiencies after being immersed in corrosive media were given in Figure 4a. The measured WCA on the PSZB surface remained above 150 and the corresponding separation efficiency was kept above 99.5% after corrosion treatment. Furthermore, residual oil contents in water for samples after being immersed in corrosive media were lower than 0.645 mg g−1, and chloroform fluxes kept stable (Figure 4b). Obviously, the WCAs and chloroform/water separation performances of the SSM-supported PSZB coatings after corrosion treatment were comparable to those of the untreated sample, demonstrating that the SSM-supported PSZB coatings maintained robust superhydrophobic characteristics under caustic conditions. The corresponding morphologies of SSM-supported PSZB coatings after corrosion treatment were displayed in Figure 5. Compared with the untreated sample (Figure 3b), the surface of PSZB coating had no significant variations after treated with HCl and NaCl as shown in Figure 5a,b. Slight dissolution was observed on the PSZB surface after treatment with 0.1 M NaOH (Figure 5c); however, there was no decrease in separation performances at all (Figure


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4), suggesting that the rough microstructure of the SSM-supported PSZB coating was not completely destroyed in this case.

Figure 4. WCAs and chloroform/water separation efficiencies (a), and chloroform fluxes and residual oil contents in water (b) of SSM-supported PSZB coatings before and after treated with corrosive media for 24 h.

Figure 5. SEM images of SSM-supported PSZB coatings after immersion in (a) 0.1 M HCl, (b) 1 M NaCl, and (c) 0.1 M NaOH for 24 h. Scale bar: 10 μm.


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The temperature may change a lot in the actual application of oil/water separation, so it is essential to evaluate the thermal stability of SSM-supported PSZB coatings. In this experiment, the samples were heated to a set temperature and kept at the temperature for 1 h. As depicted in Figure 6, the high-temperature treatment below 250 C had negligible influence on the surface wettability and chloroform/water separation performances of SSM-supported PSZB coatings during this scope. This excellent thermal stability could be attributed to the fact that the PSZB coating synthesized in a near-neutral medium containing fluoride had substantially fewer defect sites.16 However, after the heat treatment at 300 C, the WCA decreased dramatically to 136.9 and the corresponding separation efficiency dropped to 84.68%, while the residual oil content in water kept almost unchanged and the chloroform flux increased. The above results were further verified by SEM observations. As shown in Figure 7, compared with the pristine SSM-supported PSZB coating (Figure 3a), the PSZB coating maintained intact morphology after the treatment below 250 C, while it shed off from the SSM surface after being heated at 300 C (Figure 7e). This result could be interpreted by the difference of thermal expansion coefficients between the PSZB coating and the SSM


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support.24 The destruction of low-energy surface from the PSZB coating and micro/nano-scale hierarchical structure on the SSM support resulted in the disappearance of superhydrophobicity. And the detachment of the PSZB coatings gave rise to the augmented pore size of the SSM, leading to an increase in the chloroform flux. This was consistent with the changes of both WCAs and chloroform/water separation performances, which confirmed that the PSZB coating on the SSM support possessed excellent thermal stability. Furthermore, the PSZB coating could keep a close attachment on the SSM support even after high-temperature treatment below 250 C.


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Figure 6. Dependence of WCAs and chloroform/water separation efficiencies (a), and chloroform fluxes and residual oil contents in water (b) of SSM-supported PSZB coatings on high-temperature treatments.

Figure 7. SEM images of SSM-supported PSZB coatings after high-temperature treatment at (a) 100 C, (b) 150 C, (c) 200 C, (d) 250 C, and (e) 300 C for 1 h. Scale bar: 50 μm. Furthermore, the ultrasonic treatment was employed to test the adhesive strength of the PSZB coating on the substrate. The samples were immersed into chloroform solvent, followed by ultrasonic treatment. Figure 8 showed the changes in WCAs and


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chloroform/water separation performances of the SSM-supported PSZB coatings with treatment time. Although the WCA of the PSZB coating decreased slightly with treatment time, the value was still larger than 150. Meanwhile, the separation efficiencies of the SSM-supported PSZB coatings remained above 99.3% with almost constant residual oil contents in water and chloroform fluxes, suggesting that the SSMsupported PSZB coating maintained its superhydrophobicity after ultrasonic treatment for 60 min. These results would be further confirmed by SEM observations as below. As shown in Figure 9, no detachment of the PSZB coating from the support was observed. The SSM-supported PSZB coating showed the similar surface morphology to the pristine sample (Figure 3a) and maintained intact surface microstructure after ultrasonication, demonstrating robust adhesion of the PSZB coating on the substrate.


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Figure 8. WCAs and the chloroform/water separation efficiencies (a), and chloroform fluxes and residual oil contents in water (b) of SSM-supported PSZB coatings measured with respect to ultrasonic time in chloroform solvent.

Figure 9. SEM images of SSM-supported PSZB coatings after sonication for (a) 20, (b) 40, and (c) 60 min. Scale bar: 50 μm. It is noteworthy that SSM-supported PSZB coatings could be synthesized under microwave-assisted heating to substantially reduce the crystallization time.25 The template-free fabrication of zeolite-beta layers could lower the feedstock cost remarkably.26–28 The adoption of these synthesis methods might achieve an energyand cost-effective way for production of SSM-supported PSZB coatings and would be explored in the future.

4. CONCLUSIONS


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SSM-supported PSZB coatings with superhydrophobic characteristics have been fabricated by using secondary growth method. The durability and stability of the SSMsupported PSZB coating have been investigated thoroughly under various treatment conditions. The SSM-supported PSZB coating possessed excellent mechanical durability, corrosion resistance and thermal stability. It could maintain superhydrophobicity with WCAs of over 150 and exhibit high separation efficiencies of above 99% with trace amount of residual oil contents in water when exposed to abrasion, corrosive media and high-temperature environments. Meanwhile, these treatments have negligible influence on chloroform fluxes of the SSM-supported PSZB coating. In addition, the PSZB coating has shown a strong attachment to the SSM surface and retained its superhydrophobicity even after exposure to 250 C and ultrasonic environments for 1 h. It can be expected that the robust zeolite-coated SSMs with superior durability and stability would fulfill actual applications in oil/water separation.

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ASSOCIATED CONTENT


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Supporting Information Materials and Chemicals. This material is available free of charge via the Internet at http://pubs.acs.org.

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AUTHOR INFORMATION

Corresponding Author *Tel./Fax: +86 2285356517. E-mail: [email protected].

ORCID Baoquan Zhang: 0000-0001-7571-8103

Notes The authors declare no competing financial interest.

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ACKNOWLEDGMENT

We are grateful for the financial support from the National Natural Science Foundation of China (Grant No. 21136008).

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GRAPHICAL ABSTRACT


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Durability and stability of superhydrophobic stainless steel mesh

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