Facile preparation of underwater superoleophobic stainless steel mesh for oil-water separation

Facile preparation of underwater superoleophobic stainless steel mesh for oil-water separation | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Facile preparation of underwater superoleophobic stainless steel mesh for oil-water separation Yinyu Sun, Wei Yang, Changjiang Li, Zihan Yin, Caiyun Shen, Yu Liu, and 4 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6926943/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 26 Sep, 2025 Read the published version in Research on Chemical Intermediates → Version 1 posted 9 You are reading this latest preprint version Abstract Underwater superoleophobic materials have excellent underwater oil resistance due to their special wettability surface, which can cope with oil spill accidents and oily wastewater treatment. In recent years, metal-based underwater superoleophobic materials have attracted tremendous attention in the field of oil-water separation. However, the current methods for fabricating underwater superoleophobic materials have some shortcomings, such as complex preparation process, high cost, and secondary pollution. In this work, calcium carbonate nanoclusters (CaCO 3 -NCs), the product of thermal decomposition of calcium acetylacetone, were anchored on the surface of stainless steel mesh (SSM) by flame combustion method to fabricate an underwater superoleophobic material (CaCO 3 -NCs@SSM). The samples were characterized by field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectrometer (XPS), and X-ray diffractometer (XRD). These results show that CaCO 3 -NCs can be uniformly and compactly anchored on the surface of SSM by flame combustion method. Moreover, the oil-water separation capacity and the reusability of the samples were also evaluated by a self-made oil-water separation device. CaCO 3 -NCs@SSM possesses excellent underwater superoleophobic property because of its uniform and dense hydrophilic micro-nano structure on the surface, which can absorb water to form a water film. It can also be known from the contact angle test that the underwater oil contact angles of ethyl acetate, corn oil, dichloromethane, glycerol, liquid paraffin, and diesel oil on the material surface are all greater than 150°. In the oil-water separation experiment, the separation efficiencies of this material for different oil substances all exceeded 98%, among which the separation efficiency of glycerin was 99.5%. In addition, CaCO 3 -NCs@SSM maintains a separation efficiency of more than 97% over 60 consecutive cycles of oil-water separation. In summary, the underwater superoleophobic material proposed in this paper has a facile preparation method and high oil-water separation efficiency, which has great potential in solving oil spill accidents and oily wastewater treatment problems in harsh environments. underwater superoleophobic stainless steel mesh CaCO3 nanoclusters oil-water separation Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 1 Introduction A tremendous amounts of oily wastewater produced by offshore oil spills have brought great challenges to industrial economy and seriously jeopardized the ecological environment and human health [ 1 – 5 ]. It has gradually become the focus of academic and industrial communities that developing functional oil-water separation materials to deal with such problems [ 6 , 7 ]. The oil-water separation materials have high feasibility for wide application due to their advantages such as high efficiency, low cost, and great energy-saving potential in practical applications [ 8 – 10 ]. The separation principle is to allow one phase of the oil phase/water phase to pass through and repel the other phase on the other side of the separation medium. The common oil-water separation materials can be classified into superhydrophobic material [ 11 , 12 ], switchable superwettability material [ 13 , 14 ], and underwater superoleophobic material [ 15 – 18 ], which can be used to efficiently separate water-in-oil or oil-in-water mixtures[ 19 ]. Superhydrophobic materials exhibit excellent oil-water separation capabilities. However, the materials may be adhered by the oil phase during the separation process, resulting in gap blockage due to their superoleophilic. Furthermore, the clogged gaps are difficult to clean, which greatly reduces the efficiency of oil-water separation and the reusability of the materials [ 20 , 21 ]. Switchable superwettability materials have attracted increasing attention because they can switch wettability according to the needs of the application [ 22 , 23 ]. However, its preparation process is complex and the cost of raw materials is relatively high. Moreover, the switching function of the wettability will be affected during the reuse process, making it difficult for the material to accurately control the switching process [ 24 – 26 ]. The above factors have led to a relatively low possibility of the application of this material in actual production. Underwater superoleophobic materials are increasingly widely used in the oil-water separation process due to their relatively simple preparation process, high separation efficiency, and good reusability [ 27 , 28 ]. During the separation process, the excellent hydrophilicity of the underwater superoleophobic material enables water to pass through and form a water layer on its surface, effectively isolating the oil phase [ 29 ]. In addition, the preparation cost of underwater superoleophobic materials is relatively low, and there are many types of substrates to choose from [ 30 ]. All these characteristics have laid a good foundation for their wide application. Many materials are used as base materials to prepare underwater superoleophobic materials, such as cotton fabric [ 31 ], wood [ 32 ], and glass [ 33 ]. It needs to be particularly emphasized that metal mesh-based underwater superoleophobic materials have been widely studied due to their excellent mechanical properties and porous network structure, especially stainless steel mesh (SSM) [ 34 – 36 ]. The preparation principle of underwater superoleophobic SSM was obtained by changing the chemical composition or microstructure of the SSM surface [ 37 – 39 ]. Hou et al. deposited poly(diallyldimethylammonium chloride)/halloysite nanotubes coating on SSM through layer-to-layer assembly method and successfully preparing underwater superoleophobic SSM with high separation capacity [ 40 ]. Song et al. fabricated flower-structured copper benzenedicarboxylate porous clusters on SSM by solvothermal method using CuSO 4 /H 2 O 2 triggered polydopamine coating as a stable binder and nucleation layer. Moreover, the microscopic hierarchical structure of the porous cluster copper benzenedicarboxylate on SSM greatly enhances its underwater superoleophobic property [ 41 ]. Bao et al. designed an underwater superoleopic material loaded on the surface of SSM by TiO 2 /Co 3 O 4 /GO heterojunction, providing a new method for wastewater treatment in harsh environments [ 42 ]. Chen et al. combined mussel adhesion molecules (dopamine and 3,4-dihydroxy-L-phenylalanine) with the hydrophilic amphoteric monomer of sulfobetaine methacrylate through a two-step dip coating method. The material is prepared by taking advantage of the biological adhesive properties of polydopamine/poly(3,4-dihydroxy-L-phenylalanine) and the high hydrophilicity of sulfoxide methacrylate betaine to obtain underwater superolephobic SSM for oil-water separation [ 43 ]. The above-mentioned researches still have some deficiencies, such as complex preparation process, high preparation cost, and poor environmental friendliness. Therefore, it is crucial to design an SSM-based underwater superoleophobic material with a simple preparation process, low cost, and environmental friendliness for oil-water separation. This paper proposes a facile method that the in-situ anchoring of calcium carbonate nanoclusters (CaCO 3 -NCs) on the surface of SSM by the thermal decomposition reaction of calcium acetylacetone for preparing the SSM-based underwater superoleophobic material. SSM and CaCO 3 -NCs@SSM were characterized by field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectrometer (XPS), and X-ray diffractometer (XRD). In addition, performance tests such as underwater superoleophobic exploration, oil-water separation efficiency, and the reusability of the material were conducted. The results show that CaCO 3 -NCs@SSM prepared through a simple and green preparation process possesses excellent underwater superoleophobic performance, which has broad application prospects in the field of oil-water separation. 2 Materials and methods 2.1 Materials Calcium acetylacetonate (C 10 H 14 CaO 4 , 99%) and absolute ethanol were purchased from Macklin biochemical technology Co., Ltd., China (Shanghai, China). The commercial SSM of 400 meshes was purchased from Taobao (Changzhou, China). The SSM with a size of 5×5 cm was ultrasonically cleaned in ethanol for 1 h and then dried in an oven at 80 ℃ for 5 h. The reagents used in the experiment are all analytical grade reagents. 2.2 Preparation of CaCO 3 -NCs@SSM SSM was immersed in a mixed solution containing of 200 mL ethanol and 4 g of C 10 H 14 CaO 4 for 3 times to fully cover the surface of SSM and then ignited in air. This process was repeated 20 times to ensure CaCO 3 -NCs was grown on SSM (CaCO 3 -NCs@SSM). Finally, The as-obtained CaCO 3 -NCs@SSM was cleaned with deionized water and dried in 80 ℃ oven for 5 h. 2.3 Physical characterizations The morphologies of the sample suface were analyed by FESEM (Gemini 500, Zeiss, Oberkochen, Germany) and TEM (Tecnai G 2 F20, FEI, Ames, IA, USA). The surface elemental composition and distribution were determined by EDS (X-Max N 80, Oxford, UK) and XPS (ESCALAB 250Xi, Thermo Fisher, Waltham, MA, USA). X-ray diffraction patterns were recorded using an XRD apparatus equipped with a Cu Kα radiation source (D8 Advance, Bruker, Karlsruher, Germany). The static contact angles of oil under water were measured at room temperature via a contact angle meter (DSA100, KRUSS, Hamburg, Germany). 2.4 Oil-water separation and recyclability tests To evaluate the practical applications of the samples, the oil-water separation capacity was measured. CaCO 3 -NCs@SSM was fixed in a self-made oil-water separation device, and then oil and the dyed water in a 1:1 volume ratio were poured into the sand core funnel to achieve oil-water separation. The volume of water before and after separation of the mixture were V 1 and V 2 , respectively, so the oil-water separation efficiency was W = V 1 /V 2 × 100%. In the recyclability tests, it was necessary to clean and dry the samples after each use, and then conducted the next test. Results are represented as mean ± standard deviation (n = 3). 3 Results and discussion Figure 1 presents the schematic illustration of the controllable constructing process of CaCO 3 -NCs@SSM via a simple step. The SSM was immersed in a mixture of ethanol and C 10 H 14 CaO 4 , which was then removed and ignited in the air. The combustion process will release a lot of heat, so that the temperature of the reaction system continues to increase. With the increase of reaction temperature, C 10 H 14 CaO 4 was gradually oxidized to CaCO 3 [ 44 ]: C 10 H 14 CaO 4 + 11O 2 → CaCO 3 + 8CO 2 + C + 7H 2 O As the reaction progresses, CaCO 3 nanoparticles were continuously deposited on the surface of SSM. After the impregnation-combustion process was repeated for 20 times, CaCO 3 nanoparticles formed CaCO 3 -NCs with a porous micro-nano structure on the surface of SSM, which played a key role in the underwater superhydrophobicity of CaCO 3 -NCs@SSM. When water contacts the surface of CaCO 3 -NCs@SSM, water is quickly immersed into the micro-nano pores due to the good hydrophilicity of CaCO 3 , and a dense water film is formed on the surface of CaCO 3 -NCs@SSM. Therefore, when oil droplets in water come into contact with the water-wetting CaCO 3 -NCs@SSM, the oil droplets can only reach a small part of the tip of the rough structure. The main reason is that the water film is a very oleophobic medium, which isolates the direct contact between CaCO 3 -NCs@SSM and oil droplets in water [ 45 – 48 ]. Therefore, CaCO 3 -NCs@SSM cannot be adhered by oil droplets underwater, which indicates its remarkable underwater superhydrophobic property. The surface morphology of the samples was characterized by FESEM and TEM images. As shown in Fig. 2a-c, the untreated SSM has a smooth surface with a diameter of ca. 34 µm, which can be used as the substrate for the thermal decomposition reaction of C 10 H 14 CaO 4 . During the impregnation-combustion process, CaCO 3 nanoparticles were continuously generated and irregularly superimposed on the surface of SSM, eventually forming dense CaCO 3 -NCs on the surface of SSM. The diameter of the prepared CaCO 3 -NCs@SSM increased to ca. 38 µm (Fig. 2d-f). The thickness of the CaCO 3 -NCs layer growing on the surface of SSM is ca. 2 µm, which can be calculated based on the diameter difference between SSM and CaCO 3 -NCs@SSM. The hydrophilic CaCO 3 -NCs can absorb water into their porous micro-nano structure and form a water film with oleophobic properties on the surface, which can isolate CaCO 3 -NCs@SSM from oil droplets in the water. It can be seen from Fig. 3 that the TEM image clearly further confirm that the product CaCO 3 -NCs after the combustion of calcium acetylacetone is composed of the superposition of CaCO 3 nanoparticles. Furthermore, the porous micro-nano structure can be clearly observed on the surface of CaCO 3 -NCs, which provides a large specific surface area for water absorption. The surface chemical composition of the samples was characterized and analyzed by EDS and XPS. The EDS results mainly reveal the variations of C, O, and Ca elements on the surface of SSM and CaCO 3 -NCs@SSM (Fig. 4 ). The content of O element on the surface of CaCO 3 -NCs@SSM increases compared with SSM, mainly due to the reaction with oxygen in the air during combustion. It should be particularly noted that the content of Ca element on the surface of CaCO 3 -NCs@SSM is significantly higher than that on the surface of SSM. The reason for this phenomenon is that the in-situ combustion of C 10 H 14 CaO 4 on the surface of SSM to form CaCO 3 -NCs. As can be seen from the XPS results in Fig. 5, the characteristic peaks of elements C (281.44 eV) and O (531.06 eV) are clearly detected on both the surface of SSM and CaCO 3 -NCs@SSM. A new characteristic Ca peak (346.61 eV) is observed in the XPS results of CaCO 3 -NCs@SSM, and the intensity of the characteristic peak of element O is also significantly enhanced. This result further confirms that the in-situ growth of CaCO 3 nanoparticles on the SSM surface has led to an increase in the contents of Ca and O elements, which is consistent with the analysis results of EDS. As shown in Fig. 6 , XRD pattern analysis was applied to confirm the crystal structures of SSM and CaCO 3 -NCs@SSM. Compared with SSM, CaCO 3 -NCs@SSM displays dual characteristic peaks for both CaCO 3 -NCs and SSM. It can be observed that three main characteristic peaks locate at 43.6°, 50.9°, and 74.7° can be indexed to the (111), (200), and (220) lattice planes of SSM, respectively [ 49 , 50 ]. The seven new characteristic peaks at 2 θ = 22.9°, 29.3°, 35.9°, 39.4°, 43.3°, 47.4°, and 48.5° are related to the (012), (104), (110), (113), (202), (018), and (116) characteristic crystal planes of CaCO 3 , respectively [ 51 ]. Furthermore, the characteristic peaks located at the (111), (200), and (220) lattice plane of CaCO 3 -NCs@SSM were weakened compared with those of SSM, further confirming that the surface of SSM was uniformly and densely covered by the CaCO 3 -NCs layer after impregnation and combustion treatment. The confirmatory experiments were conducted to further evaluate and analyze the underwater superoleophobic properties of SSM and CaCO 3 -NCs@SSM. As shown in Fig. 7 , when water was added to the dichloromethane solution stained with 4-(4-Nitrophenylazo)-1-naphthol, the aqueous phase and the oil phase appeared to separate. The water layer was on top and the oil layer was at the bottom because the density of dichloromethane is greater than that of water. Then SSM and CaCO 3 -NCs@SSM were placed in the aqueous solution and both sank to the oil-water interface, mainly because SSM and CaCO 3 -NCs@SSM both possess good hydrophilicity. An interesting phenomenon was that both SSM and CaCO 3 -NCs@SSM were suspended at the oil-water interface. The reason is that SSM and CaCO 3 -NCs@SSM are both wetted by water and formed water films on their surfaces, which give them hydrophobic underwater properties. To further observe the underwater superoleophobic performance, the samples were pressed into the oil phase. It can be clearly seen from Fig. 7 a that SSM sank to the bottom of the beaker in a relatively short time after coming into contact with the dichloromethane solution, which indicates that the water film of SSM is replaced by the oil phase and makes SSM exhibit lipophilicity. However, when CaCO 3 -NCs@SSM was pressed into the oil phase and then released, the sample quickly floated up to the oil-water interface, suggesting that the water film formed by the micro-nano structures on the CaCO 3 -NCs@SSM surface in the water can effectively isolate the oil phase (Fig. 7 b). The above phenomenon demonstrates that CaCO 3 -NCs@SSM exhibits good hydrophilicity and superoleophobicity underwater. Rolling experiments of oil droplets in water further visually demonstrate the underwater superoleophobic properties of CaCO 3 -NCs@SSM. The solvents used in this experiment were liquid paraffin with a density less than that of water and dichloromethane with a density greater than that of water, respectively. To facilitate the observation of the phenomenon, they were all stained with 4-(4-Nitrophenylazo)-1-naphthol. As shown in Fig. 8 , it should be particularly noted that when conducting the oil drop rolling experiment in water with liquid paraffin, the syringe needle needed to be bent and the solvent injected from the bottom of the material. To better show the rolling trajectory of the droplet, CaCO 3 -NCs@SSM was folded into an "L" shape. When dichloromethane was used as the solvent, dichloromethane was directly injected into the sample surface and the rolling trajectory of the oil droplets was observed. Figure 8 (a) shows that liquid paraffin rolled upward along the inclined plane of the material under the action of buoyancy to the corner of the "L" shape and suspended there. Then the inclination angle of the material was adjusted by turning the tweezers, and the oil droplets continued to rise steadily from the corner to the water surface. In Fig. 8 (b), dichloromethane rolled along the material surface to the bottom of the beaker under the action of gravity. Neither of the two solvents of different densities show oil droplet adhesion to the material, which further indicates that CaCO 3 -NCs@SSM has low underwater oil adhesion, resulting in excellent underwater superoleophobic properties. To further quantitatively evaluate the underwater superoleophobic properties of CaCO 3 -NCs@SSM, the underwater oil contact angles of ethyl acetate, corn oil, dichloromethane, glycerin, liquid paraffin, and diesel oil on its surface were tested (Fig. 9 ). It can be seen that the underwater oil contact angles of oil substances are greater than 150°, especially that of corn oil reaches 155.9°. Figure 9 shows that the underwater oil droplets on the material surface are nearly spherical. The reason for this phenomenon is that the superhydrophilic micro-nano structures of CaCO 3 -NCs@SSM trap water and form a water film, which is a extremely repellent medium, resulting in an extremely high water-oil contact angle. When oil droplets come into contact with the material surface underwater, the water film can effectively reduce the contact area between the material and the oil droplets. Therefore, the oil droplets remain nearly spherical and have the large contact angles on the CaCO 3 -NCs@SSM surface in water. To better understand the underwater superoleophobic mechanism of this material from a theoretical perspective, the solid-oil-water wetting model was explored and analyzed by Fig. 10 . During the oil-water separation process, the oil-water separation material is subjected to the pressure generated by gravity, which is called intrusion pressure (P i ). When the intrusion pressure exceeds the pressure range, oil (or water) can penetrate through the material, thereby reducing the separation effect. Therefore, the intrusion pressure is a key parameter in the oil-water separation device. The theoretical intrusion pressure can be formulated as [ 52 , 53 ]: P i = 2s / R = -4s cosθ i / l Where s is the surface tension, R is the radius of the meniscus, θ i is the contact angle on the surface, and l is the distance between two micropores. According to this formula, it can be known that when θ i is less than 90° (the intrusion pressure P i 0), the liquid will gradually permeate through the oil-water separation material. Based on the above analysis, the contact angle of water on the surface of CaCO 3 -NCs@SSM material in the air is 0°, so water can pass through CaCO 3 -NCs@SSM rapidly under the action of intrusion pressure. The contact angle of oil substances on the pre-wetted surface of CaCO 3 -NCs@SSM all exceeds 150°, the material can repulse the penetration of oil substances. This theory further indicates that underwater superoleophobic CaCO 3 -NCs@SSM will possess great potential in the field of oil-water separation. Underwater superhydrophobic materials have important application prospects in the field of efficient oil-water separation. Therefore, a self-made oil-water separation device was used to test the oil-water separation efficiency of CaCO 3 -NCs@SSM material, as shown in Fig. 11 . Firstly, CaCO 3 -NCs@SSM was fixed in the oil-water separator and then pre-wetted with water. Secondly, the aqueous solution stained with methyl blue and corn oil were poured into the sand core funnel at a ratio of 1:1 (v/v). The methyl blue aqueous solution passed through CaCO 3 -NCs@SSM and flowed into the conical flask, while the corn oil was isolated at the top of the material. The reason for this phenomenon is that the underwater superoleophobic CaCO 3 -NCs@SSM with a dense micro-nano structure is pre-wetted to form a water film on its surface, which enables the oil phase to be isolated, while the water phase rapidly passes through the material under the action of gravity, achieving oil-water separation. Finally, the oil-water separation efficiency of the material can be calculated based on the volume of water before and after separation. Moreover, no obvious residual mixed liquid was observed in either the oil phase or the water phase after separation, which intuitively demonstrates the high oil-water separation efficiency of the material. In the practical application process, the separation efficiency of materials for different oil substances and the reusability of materials are both of crucial importance. Figure 12 shows that CaCO 3 -NCs@SSM can achieve the separation efficiencies of over 98% for four kinds of light oils (ethyl acetate, corn oil, liquid paraffin, and diesel oil) and two kinds of heavy oils (dichloromethane and glycerin). For the oil-water mixture with glycerol as the oil phase, the separation efficiency of the material can reach 99.5%. In addition, the reusability experiment of CaCO 3 -NCs@SSM was conducted using the glycerin-water mixture. After 60 cycles of oil-water separation, the used CaCO 3 -NCs@SSM still maintained stable oil-water separation efficiency of over 97% for glycerin. To sum up, the superhydrophilic and underwater superoleophobic CaCO 3 -NCs@SSM material prepared by simple and effective methods have great prospects for efficient oil-water separation. 4 Conclusions In conclusion, the underwater superoleophobic material based on SSM was successfully prepared by a facile and environmentally friendly in-situ flame method. By loading uniform and dense CaCO 3 -NCs onto the surface of the original substrate SSM, the material not only has superhydrophilicity in the air, but also the underwater contact angles of different oil substances all reach more than 150°, indicating that the material possesses underwater superoleophobic properties. This special wettability enables CaCO 3 -NCs@SSM to separate oil and water mixtures completely by gravity. The results of the sample performance test and characterization analysis show that the separation efficiency of this material for different oil substances can be maintained above 98%, and there is no obvious downward trend in its separation efficiency for glycerol after being reused 60 times. The micro-nano structure on the surface of the material enables it to form a water film underwater, thereby endowing the material with high self-cleaning property and anti-fouling performance. Therefore, this material holds great potential for the treatment of purifying oil-water mixtures and collecting oil pollutants from underwater environments. Declarations Acknowledgments This work was supported by Anhui Nature Science Research Program (Grant No. 2022AH051954), Huangshan University Science Research Program (Grant No. 2022xkjzd001), Youth Teacher Training Action Project of Anhui Province (DTR2023046). Author contributions All authors have contributed to the research conception and design. The material preparation, data collection, and initial draft of the manuscript were carried out by Yinyu Sun and Caiyun Shen. The analysis of data and the drawing of charts were carried out by Wei Yang, Zihan Yin, Yu Liu, Qi Chen, Qing Ding, and Qiaoqiao Zhang. Changjiang Li and Zhongcheng Ke proofread the entire paper. All authors have provided comments on previous versions of the manuscript. All authors have read and approved the final manuscript. Conflicts of interest or competing interests The authors declare that they have no known competing financial interests or personal relationships. Data and code availability Not Applicable Supplementary information Not Applicable Ethical approval Not Applicable References J.F. Xi, S. Jiang, Y.L. Lou, H.Q. Dai, W.B. Wu, Cellulose. 28 , 1 (2021) J. Zhao, X.Y. Chen, Y.H. Zhou, H.J. Tian, Q.J. Guo, X.D. Hu, Research on Chemical Intermediates. 46 , 1805 (2020) J.J. Wang, L.M. Wang, Journal of Materials Research. 35 , 1 (2020) Y.W. Cui, X.D. 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Singh, ACS Applied Materials & Interfaces. 9 , 6007 (2017) L. Biao, F.F. Lange, Journal of Colloid and Interface Science. 298 , 899 (2006) Additional Declarations No competing interests reported. Cite Share Download PDF Status: Published Journal Publication published 26 Sep, 2025 Read the published version in Research on Chemical Intermediates → Version 1 posted Editorial decision: Revision requested 29 Jul, 2025 Reviews received at journal 29 Jul, 2025 Reviews received at journal 23 Jul, 2025 Reviewers agreed at journal 23 Jul, 2025 Reviewers agreed at journal 11 Jul, 2025 Reviewers invited by journal 09 Jul, 2025 Editor assigned by journal 19 Jun, 2025 Submission checks completed at journal 19 Jun, 2025 First submitted to journal 18 Jun, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6926943","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":483822224,"identity":"3db8bfbe-8ac1-4d3e-bfc9-cc6e21f0ae2c","order_by":0,"name":"Yinyu Sun","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Yinyu","middleName":"","lastName":"Sun","suffix":""},{"id":483822225,"identity":"ea6641f8-3425-4c22-a75a-c8e890ea4cd0","order_by":1,"name":"Wei Yang","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Wei","middleName":"","lastName":"Yang","suffix":""},{"id":483822226,"identity":"376aad98-bc3f-4928-b186-b044629c5823","order_by":2,"name":"Changjiang Li","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAqElEQVRIiWNgGAWjYBACNvb2gwcSGNjkgIwDxGnh4zmTANJiDGIQp0VOwsEAZHriPCCDSIdJMCQceFDDl94GZDD8qNhGhBbpxgMHEo6x5bYBGYw9Z24ToUXmQMKBxAagFiCDmbGNGC0SCQYgLekgBmlaEkjQAg7kY2yGbUDGQaL8It/efvDhj5pj8iDGgx8VRGiBgmNg8gDR6oGghhTFo2AUjIJRMNIAAFTIPShPzpO/AAAAAElFTkSuQmCC","orcid":"","institution":"Huangshan University","correspondingAuthor":true,"prefix":"","firstName":"Changjiang","middleName":"","lastName":"Li","suffix":""},{"id":483822227,"identity":"5c7bb664-1d8b-41f8-91d5-72ede33cfd18","order_by":3,"name":"Zihan Yin","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Zihan","middleName":"","lastName":"Yin","suffix":""},{"id":483822228,"identity":"afdd3ca4-5a55-4c45-a308-7eaaf935d08f","order_by":4,"name":"Caiyun Shen","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Caiyun","middleName":"","lastName":"Shen","suffix":""},{"id":483822229,"identity":"114b0a46-7452-4edc-afc5-3988d88aea95","order_by":5,"name":"Yu Liu","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Yu","middleName":"","lastName":"Liu","suffix":""},{"id":483822230,"identity":"7475377d-e8eb-4a3a-b951-376c301227c8","order_by":6,"name":"Qi Chen","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Qi","middleName":"","lastName":"Chen","suffix":""},{"id":483822231,"identity":"3b8bfe08-9e50-4dae-b0a6-821efd1f8d67","order_by":7,"name":"Qing Ding","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Qing","middleName":"","lastName":"Ding","suffix":""},{"id":483822232,"identity":"50f6ac32-0cdd-4cc3-aafe-e532f1d423c9","order_by":8,"name":"Qiaoqiao Zhang","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Qiaoqiao","middleName":"","lastName":"Zhang","suffix":""},{"id":483822233,"identity":"721cbfb9-4e75-4cc4-ac26-96978d152540","order_by":9,"name":"Zhongcheng Ke","email":"","orcid":"","institution":"Huangshan University","correspondingAuthor":false,"prefix":"","firstName":"Zhongcheng","middleName":"","lastName":"Ke","suffix":""}],"badges":[],"createdAt":"2025-06-19 03:08:17","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6926943/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6926943/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s11164-025-05757-4","type":"published","date":"2025-09-26T15:58:15+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":86643478,"identity":"05cd2bd9-49ff-46e1-89b3-045ba46ff46b","added_by":"auto","created_at":"2025-07-14 08:36:38","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":221775,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic illustration of the preparation of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM\u003c/p\u003e","description":"","filename":"image1.png","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/55bd2c7fda6224cac6f41b00.png"},{"id":86646531,"identity":"f26eaa89-aab2-4dac-bc24-111302c97693","added_by":"auto","created_at":"2025-07-14 09:00:39","extension":"jpeg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":182298,"visible":true,"origin":"","legend":"\u003cp\u003eFESEM images of SSM (a-c) and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM (d-f)\u003c/p\u003e","description":"","filename":"image2.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/d854a666980e321a3a28afa2.jpeg"},{"id":86643474,"identity":"5aeaff95-8e4d-4825-ad55-4d07fe444697","added_by":"auto","created_at":"2025-07-14 08:36:38","extension":"jpeg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":57482,"visible":true,"origin":"","legend":"\u003cp\u003eTEM images of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs\u003c/p\u003e","description":"","filename":"image3.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/0d04c9f3bbda9265c5b3dcbb.jpeg"},{"id":86643496,"identity":"aa40020c-1520-42fe-b1da-dddcec486429","added_by":"auto","created_at":"2025-07-14 08:36:39","extension":"jpeg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":94437,"visible":true,"origin":"","legend":"\u003cp\u003e(a) EDS elemental mappings of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM ; (b) EDS spectra of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM.\u003c/p\u003e","description":"","filename":"image4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/45908b4eaf0340530bd03e3a.jpeg"},{"id":86643486,"identity":"0b30bab6-388f-4c38-9d88-e904d2a475fe","added_by":"auto","created_at":"2025-07-14 08:36:38","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":282374,"visible":true,"origin":"","legend":"\u003cp\u003eXPS analysis of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM.\u003c/p\u003e","description":"","filename":"image5.png","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/aff871368fa9c2e9bfa4c9df.png"},{"id":86643475,"identity":"2f3fe06d-e5c2-41c0-8363-527585e2d610","added_by":"auto","created_at":"2025-07-14 08:36:38","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":231979,"visible":true,"origin":"","legend":"\u003cp\u003eXRD analysis of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM.\u003c/p\u003e","description":"","filename":"image6.png","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/72ab5f3881d65d3d581c7d3f.png"},{"id":86643492,"identity":"25d31a7c-df3d-4b75-bba2-d62883b975d7","added_by":"auto","created_at":"2025-07-14 08:36:39","extension":"jpeg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":80099,"visible":true,"origin":"","legend":"\u003cp\u003ePhotographs of SSM(a) and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM(b) floating test in an dichloromethane-water mixture\u003c/p\u003e","description":"","filename":"image7.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/edbad7491a1097674a77bcd7.jpeg"},{"id":86643501,"identity":"5abc2018-6807-4e67-8292-37b0057f1bb6","added_by":"auto","created_at":"2025-07-14 08:36:39","extension":"jpeg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":64495,"visible":true,"origin":"","legend":"\u003cp\u003ePhotographs of the underwater oil rolling test on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM (a: liquid paraffin; b: dichloromethane)\u003c/p\u003e","description":"","filename":"image8.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/6bbfcb8e3f5e9ef840d52e1e.jpeg"},{"id":86643502,"identity":"0b39d0dc-64b6-4437-b483-4b21c25164ef","added_by":"auto","created_at":"2025-07-14 08:36:39","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":56378,"visible":true,"origin":"","legend":"\u003cp\u003eUnderwater contact angles of different oil substances on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. Results are represented as mean ± standard deviation (n = 3).\u003c/p\u003e","description":"","filename":"image9.png","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/83dd592b5c8dc18751f4b375.png"},{"id":86644749,"identity":"326111fe-20b0-4d1c-bb40-230810297586","added_by":"auto","created_at":"2025-07-14 08:44:39","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":101893,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic diagrams of the solid-oil-water wetting model. (a) Water can permeate through CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM due to \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003ei \u003c/em\u003e\u003c/sub\u003e\u003cem\u003e\u0026lt;\u003c/em\u003e\u003csub\u003e\u003cem\u003e \u003c/em\u003e\u003c/sub\u003e0; (b) Oil substance cannot pass through CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM due to \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003ei \u003c/em\u003e\u003c/sub\u003e\u003cem\u003e\u0026gt;\u003c/em\u003e\u003csub\u003e\u003cem\u003e \u003c/em\u003e\u003c/sub\u003e0.\u003c/p\u003e","description":"","filename":"image10.png","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/e0580e282e5a10031e5a994c.png"},{"id":86643488,"identity":"9821d9de-c6ec-441c-8aaf-f4605c386c63","added_by":"auto","created_at":"2025-07-14 08:36:39","extension":"jpeg","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":52897,"visible":true,"origin":"","legend":"\u003cp\u003eGravity-driven separation test for the corn oil-water mixture was performed via CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM.\u003c/p\u003e","description":"","filename":"image11.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/0f651de488216e4cff8889cc.jpeg"},{"id":86643493,"identity":"db33f618-b6a8-42e5-a86a-120dbb6014d5","added_by":"auto","created_at":"2025-07-14 08:36:39","extension":"png","order_by":12,"title":"Figure 12","display":"","copyAsset":false,"role":"figure","size":830488,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Oil-water separation efficiency of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM for different oil substances; (b) Recyclability test of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM for glycerin. Results are represented as mean ± standard deviation (n = 3).\u003c/p\u003e","description":"","filename":"image12.png","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/c330776422198aeb28fab815.png"},{"id":92430668,"identity":"c8f45d6c-8cf6-42ce-bd65-cd1e1f7a8633","added_by":"auto","created_at":"2025-09-29 16:07:30","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2784154,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6926943/v1/eae15403-407b-451e-bdfe-ce8db0ce6d13.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Facile preparation of underwater superoleophobic stainless steel mesh for oil-water separation","fulltext":[{"header":"1 Introduction","content":"\u003cp\u003eA tremendous amounts of oily wastewater produced by offshore oil spills have brought great challenges to industrial economy and seriously jeopardized the ecological environment and human health [\u003cspan additionalcitationids=\"CR2 CR3 CR4\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. It has gradually become the focus of academic and industrial communities that developing functional oil-water separation materials to deal with such problems [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e, \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. The oil-water separation materials have high feasibility for wide application due to their advantages such as high efficiency, low cost, and great energy-saving potential in practical applications [\u003cspan additionalcitationids=\"CR9\" citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. The separation principle is to allow one phase of the oil phase/water phase to pass through and repel the other phase on the other side of the separation medium. The common oil-water separation materials can be classified into superhydrophobic material [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e, \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e], switchable superwettability material [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e], and underwater superoleophobic material [\u003cspan additionalcitationids=\"CR16 CR17\" citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e], which can be used to efficiently separate water-in-oil or oil-in-water mixtures[\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. Superhydrophobic materials exhibit excellent oil-water separation capabilities. However, the materials may be adhered by the oil phase during the separation process, resulting in gap blockage due to their superoleophilic. Furthermore, the clogged gaps are difficult to clean, which greatly reduces the efficiency of oil-water separation and the reusability of the materials [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e, \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. Switchable superwettability materials have attracted increasing attention because they can switch wettability according to the needs of the application [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e, \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. However, its preparation process is complex and the cost of raw materials is relatively high. Moreover, the switching function of the wettability will be affected during the reuse process, making it difficult for the material to accurately control the switching process [\u003cspan additionalcitationids=\"CR25\" citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. The above factors have led to a relatively low possibility of the application of this material in actual production. Underwater superoleophobic materials are increasingly widely used in the oil-water separation process due to their relatively simple preparation process, high separation efficiency, and good reusability [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. During the separation process, the excellent hydrophilicity of the underwater superoleophobic material enables water to pass through and form a water layer on its surface, effectively isolating the oil phase [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. In addition, the preparation cost of underwater superoleophobic materials is relatively low, and there are many types of substrates to choose from [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. All these characteristics have laid a good foundation for their wide application.\u003c/p\u003e\u003cp\u003eMany materials are used as base materials to prepare underwater superoleophobic materials, such as cotton fabric [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e], wood [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e], and glass [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e]. It needs to be particularly emphasized that metal mesh-based underwater superoleophobic materials have been widely studied due to their excellent mechanical properties and porous network structure, especially stainless steel mesh (SSM) [\u003cspan additionalcitationids=\"CR35\" citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. The preparation principle of underwater superoleophobic SSM was obtained by changing the chemical composition or microstructure of the SSM surface [\u003cspan additionalcitationids=\"CR38\" citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]. Hou et al. deposited poly(diallyldimethylammonium chloride)/halloysite nanotubes coating on SSM through layer-to-layer assembly method and successfully preparing underwater superoleophobic SSM with high separation capacity [\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]. Song et al. fabricated flower-structured copper benzenedicarboxylate porous clusters on SSM by solvothermal method using CuSO\u003csub\u003e4\u003c/sub\u003e/H\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e2\u003c/sub\u003e triggered polydopamine coating as a stable binder and nucleation layer. Moreover, the microscopic hierarchical structure of the porous cluster copper benzenedicarboxylate on SSM greatly enhances its underwater superoleophobic property [\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e]. Bao et al. designed an underwater superoleopic material loaded on the surface of SSM by TiO\u003csub\u003e2\u003c/sub\u003e/Co\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e/GO heterojunction, providing a new method for wastewater treatment in harsh environments [\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e]. Chen et al. combined mussel adhesion molecules (dopamine and 3,4-dihydroxy-L-phenylalanine) with the hydrophilic amphoteric monomer of sulfobetaine methacrylate through a two-step dip coating method. The material is prepared by taking advantage of the biological adhesive properties of polydopamine/poly(3,4-dihydroxy-L-phenylalanine) and the high hydrophilicity of sulfoxide methacrylate betaine to obtain underwater superolephobic SSM for oil-water separation [\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. The above-mentioned researches still have some deficiencies, such as complex preparation process, high preparation cost, and poor environmental friendliness. Therefore, it is crucial to design an SSM-based underwater superoleophobic material with a simple preparation process, low cost, and environmental friendliness for oil-water separation.\u003c/p\u003e\u003cp\u003eThis paper proposes a facile method that the in-situ anchoring of calcium carbonate nanoclusters (CaCO\u003csub\u003e3\u003c/sub\u003e-NCs) on the surface of SSM by the thermal decomposition reaction of calcium acetylacetone for preparing the SSM-based underwater superoleophobic material. SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM were characterized by field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectrometer (XPS), and X-ray diffractometer (XRD). In addition, performance tests such as underwater superoleophobic exploration, oil-water separation efficiency, and the reusability of the material were conducted. The results show that CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM prepared through a simple and green preparation process possesses excellent underwater superoleophobic performance, which has broad application prospects in the field of oil-water separation.\u003c/p\u003e"},{"header":"2 Materials and methods","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e\u003ch2\u003e2.1 Materials\u003c/h2\u003e\u003cp\u003eCalcium acetylacetonate (C\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e, 99%) and absolute ethanol were purchased from Macklin biochemical technology Co., Ltd., China (Shanghai, China). The commercial SSM of 400 meshes was purchased from Taobao (Changzhou, China). The SSM with a size of 5\u0026times;5 cm was ultrasonically cleaned in ethanol for 1 h and then dried in an oven at 80 ℃ for 5 h. The reagents used in the experiment are all analytical grade reagents.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec4\" class=\"Section2\"\u003e\u003ch2\u003e2.2 Preparation of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM\u003c/h2\u003e\u003cp\u003eSSM was immersed in a mixed solution containing of 200 mL ethanol and 4 g of C\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e for 3 times to fully cover the surface of SSM and then ignited in air. This process was repeated 20 times to ensure CaCO\u003csub\u003e3\u003c/sub\u003e-NCs was grown on SSM (CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM). Finally, The as-obtained CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM was cleaned with deionized water and dried in 80 ℃ oven for 5 h.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec5\" class=\"Section2\"\u003e\u003ch2\u003e2.3 Physical characterizations\u003c/h2\u003e\u003cp\u003eThe morphologies of the sample suface were analyed by FESEM (Gemini 500, Zeiss, Oberkochen, Germany) and TEM (Tecnai G\u003csup\u003e2\u003c/sup\u003e F20, FEI, Ames, IA, USA). The surface elemental composition and distribution were determined by EDS (X-Max\u003csup\u003eN\u003c/sup\u003e 80, Oxford, UK) and XPS (ESCALAB 250Xi, Thermo Fisher, Waltham, MA, USA). X-ray diffraction patterns were recorded using an XRD apparatus equipped with a Cu Kα radiation source (D8 Advance, Bruker, Karlsruher, Germany). The static contact angles of oil under water were measured at room temperature via a contact angle meter (DSA100, KRUSS, Hamburg, Germany).\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec6\" class=\"Section2\"\u003e\u003ch2\u003e2.4 Oil-water separation and recyclability tests\u003c/h2\u003e\u003cp\u003eTo evaluate the practical applications of the samples, the oil-water separation capacity was measured. CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM was fixed in a self-made oil-water separation device, and then oil and the dyed water in a 1:1 volume ratio were poured into the sand core funnel to achieve oil-water separation. The volume of water before and after separation of the mixture were V\u003csub\u003e1\u003c/sub\u003e and V\u003csub\u003e2\u003c/sub\u003e, respectively, so the oil-water separation efficiency was W\u0026thinsp;=\u0026thinsp;V\u003csub\u003e1\u003c/sub\u003e/V\u003csub\u003e2\u003c/sub\u003e \u0026times; 100%. In the recyclability tests, it was necessary to clean and dry the samples after each use, and then conducted the next test. Results are represented as mean\u0026thinsp;\u0026plusmn;\u0026thinsp;standard deviation (n\u0026thinsp;=\u0026thinsp;3).\u003c/p\u003e\u003c/div\u003e"},{"header":"3 Results and discussion","content":"\u003cp\u003eFigure 1 presents the schematic illustration of the controllable constructing process of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM via a simple step. The SSM was immersed in a mixture of ethanol and C\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e, which was then removed and ignited in the air. The combustion process will release a lot of heat, so that the temperature of the reaction system continues to increase. With the increase of reaction temperature, C\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e was gradually oxidized to CaCO\u003csub\u003e3\u003c/sub\u003e [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e]:\u003c/p\u003e\u003cp\u003eC\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e\u0026thinsp;+\u0026thinsp;11O\u003csub\u003e2\u003c/sub\u003e \u0026rarr; CaCO\u003csub\u003e3\u003c/sub\u003e\u0026thinsp;+\u0026thinsp;8CO\u003csub\u003e2\u003c/sub\u003e\u0026thinsp;+\u0026thinsp;C\u0026thinsp;+\u0026thinsp;7H\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e\u003cp\u003eAs the reaction progresses, CaCO\u003csub\u003e3\u003c/sub\u003e nanoparticles were continuously deposited on the surface of SSM. After the impregnation-combustion process was repeated for 20 times, CaCO\u003csub\u003e3\u003c/sub\u003e nanoparticles formed CaCO\u003csub\u003e3\u003c/sub\u003e-NCs with a porous micro-nano structure on the surface of SSM, which played a key role in the underwater superhydrophobicity of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. When water contacts the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM, water is quickly immersed into the micro-nano pores due to the good hydrophilicity of CaCO\u003csub\u003e3\u003c/sub\u003e, and a dense water film is formed on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. Therefore, when oil droplets in water come into contact with the water-wetting CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM, the oil droplets can only reach a small part of the tip of the rough structure. The main reason is that the water film is a very oleophobic medium, which isolates the direct contact between CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM and oil droplets in water [\u003cspan additionalcitationids=\"CR46 CR47\" citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e]. Therefore, CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM cannot be adhered by oil droplets underwater, which indicates its remarkable underwater superhydrophobic property.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe surface morphology of the samples was characterized by FESEM and TEM images. As shown in Fig.\u0026nbsp;2a-c, the untreated SSM has a smooth surface with a diameter of ca. 34 \u0026micro;m, which can be used as the substrate for the thermal decomposition reaction of C\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e. During the impregnation-combustion process, CaCO\u003csub\u003e3\u003c/sub\u003e nanoparticles were continuously generated and irregularly superimposed on the surface of SSM, eventually forming dense CaCO\u003csub\u003e3\u003c/sub\u003e-NCs on the surface of SSM. The diameter of the prepared CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM increased to ca. 38 \u0026micro;m (Fig.\u0026nbsp;2d-f). The thickness of the CaCO\u003csub\u003e3\u003c/sub\u003e-NCs layer growing on the surface of SSM is ca. 2 \u0026micro;m, which can be calculated based on the diameter difference between SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. The hydrophilic CaCO\u003csub\u003e3\u003c/sub\u003e-NCs can absorb water into their porous micro-nano structure and form a water film with oleophobic properties on the surface, which can isolate CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM from oil droplets in the water. It can be seen from Fig.\u0026nbsp;3 that the TEM image clearly further confirm that the product CaCO\u003csub\u003e3\u003c/sub\u003e-NCs after the combustion of calcium acetylacetone is composed of the superposition of CaCO\u003csub\u003e3\u003c/sub\u003e nanoparticles. Furthermore, the porous micro-nano structure can be clearly observed on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs, which provides a large specific surface area for water absorption.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe surface chemical composition of the samples was characterized and analyzed by EDS and XPS. The EDS results mainly reveal the variations of C, O, and Ca elements on the surface of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e4\u003c/span\u003e). The content of O element on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM increases compared with SSM, mainly due to the reaction with oxygen in the air during combustion. It should be particularly noted that the content of Ca element on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM is significantly higher than that on the surface of SSM. The reason for this phenomenon is that the in-situ combustion of C\u003csub\u003e10\u003c/sub\u003eH\u003csub\u003e14\u003c/sub\u003eCaO\u003csub\u003e4\u003c/sub\u003e on the surface of SSM to form CaCO\u003csub\u003e3\u003c/sub\u003e-NCs. As can be seen from the XPS results in Fig.\u0026nbsp;5, the characteristic peaks of elements C (281.44 eV) and O (531.06 eV) are clearly detected on both the surface of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. A new characteristic Ca peak (346.61 eV) is observed in the XPS results of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM, and the intensity of the characteristic peak of element O is also significantly enhanced. This result further confirms that the in-situ growth of CaCO\u003csub\u003e3\u003c/sub\u003e nanoparticles on the SSM surface has led to an increase in the contents of Ca and O elements, which is consistent with the analysis results of EDS.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eAs shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e6\u003c/span\u003e, XRD pattern analysis was applied to confirm the crystal structures of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. Compared with SSM, CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM displays dual characteristic peaks for both CaCO\u003csub\u003e3\u003c/sub\u003e-NCs and SSM. It can be observed that three main characteristic peaks locate at 43.6\u0026deg;, 50.9\u0026deg;, and 74.7\u0026deg; can be indexed to the (111), (200), and (220) lattice planes of SSM, respectively [\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e, \u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e]. The seven new characteristic peaks at 2\u003cem\u003eθ\u003c/em\u003e\u0026thinsp;=\u0026thinsp;22.9\u0026deg;, 29.3\u0026deg;, 35.9\u0026deg;, 39.4\u0026deg;, 43.3\u0026deg;, 47.4\u0026deg;, and 48.5\u0026deg; are related to the (012), (104), (110), (113), (202), (018), and (116) characteristic crystal planes of CaCO\u003csub\u003e3\u003c/sub\u003e, respectively [\u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e51\u003c/span\u003e]. Furthermore, the characteristic peaks located at the (111), (200), and (220) lattice plane of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM were weakened compared with those of SSM, further confirming that the surface of SSM was uniformly and densely covered by the CaCO\u003csub\u003e3\u003c/sub\u003e-NCs layer after impregnation and combustion treatment.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe confirmatory experiments were conducted to further evaluate and analyze the underwater superoleophobic properties of SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e7\u003c/span\u003e, when water was added to the dichloromethane solution stained with 4-(4-Nitrophenylazo)-1-naphthol, the aqueous phase and the oil phase appeared to separate. The water layer was on top and the oil layer was at the bottom because the density of dichloromethane is greater than that of water. Then SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM were placed in the aqueous solution and both sank to the oil-water interface, mainly because SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM both possess good hydrophilicity. An interesting phenomenon was that both SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM were suspended at the oil-water interface. The reason is that SSM and CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM are both wetted by water and formed water films on their surfaces, which give them hydrophobic underwater properties. To further observe the underwater superoleophobic performance, the samples were pressed into the oil phase. It can be clearly seen from Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e7\u003c/span\u003ea that SSM sank to the bottom of the beaker in a relatively short time after coming into contact with the dichloromethane solution, which indicates that the water film of SSM is replaced by the oil phase and makes SSM exhibit lipophilicity. However, when CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM was pressed into the oil phase and then released, the sample quickly floated up to the oil-water interface, suggesting that the water film formed by the micro-nano structures on the CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM surface in the water can effectively isolate the oil phase (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e7\u003c/span\u003eb). The above phenomenon demonstrates that CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM exhibits good hydrophilicity and superoleophobicity underwater.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eRolling experiments of oil droplets in water further visually demonstrate the underwater superoleophobic properties of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM. The solvents used in this experiment were liquid paraffin with a density less than that of water and dichloromethane with a density greater than that of water, respectively. To facilitate the observation of the phenomenon, they were all stained with 4-(4-Nitrophenylazo)-1-naphthol. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e8\u003c/span\u003e, it should be particularly noted that when conducting the oil drop rolling experiment in water with liquid paraffin, the syringe needle needed to be bent and the solvent injected from the bottom of the material. To better show the rolling trajectory of the droplet, CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM was folded into an \"L\" shape. When dichloromethane was used as the solvent, dichloromethane was directly injected into the sample surface and the rolling trajectory of the oil droplets was observed. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e8\u003c/span\u003e (a) shows that liquid paraffin rolled upward along the inclined plane of the material under the action of buoyancy to the corner of the \"L\" shape and suspended there. Then the inclination angle of the material was adjusted by turning the tweezers, and the oil droplets continued to rise steadily from the corner to the water surface. In Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e8\u003c/span\u003e (b), dichloromethane rolled along the material surface to the bottom of the beaker under the action of gravity. Neither of the two solvents of different densities show oil droplet adhesion to the material, which further indicates that CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM has low underwater oil adhesion, resulting in excellent underwater superoleophobic properties.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eTo further quantitatively evaluate the underwater superoleophobic properties of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM, the underwater oil contact angles of ethyl acetate, corn oil, dichloromethane, glycerin, liquid paraffin, and diesel oil on its surface were tested (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e9\u003c/span\u003e). It can be seen that the underwater oil contact angles of oil substances are greater than 150\u0026deg;, especially that of corn oil reaches 155.9\u0026deg;. Figure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e9\u003c/span\u003e shows that the underwater oil droplets on the material surface are nearly spherical. The reason for this phenomenon is that the superhydrophilic micro-nano structures of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM trap water and form a water film, which is a extremely repellent medium, resulting in an extremely high water-oil contact angle. When oil droplets come into contact with the material surface underwater, the water film can effectively reduce the contact area between the material and the oil droplets. Therefore, the oil droplets remain nearly spherical and have the large contact angles on the CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM surface in water.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eTo better understand the underwater superoleophobic mechanism of this material from a theoretical perspective, the solid-oil-water wetting model was explored and analyzed by Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e10\u003c/span\u003e. During the oil-water separation process, the oil-water separation material is subjected to the pressure generated by gravity, which is called intrusion pressure (P\u003csub\u003ei\u003c/sub\u003e). When the intrusion pressure exceeds the pressure range, oil (or water) can penetrate through the material, thereby reducing the separation effect. Therefore, the intrusion pressure is a key parameter in the oil-water separation device. The theoretical intrusion pressure can be formulated as [\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e, \u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e53\u003c/span\u003e]:\u003c/p\u003e\u003cp\u003e\u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e \u003cem\u003e= 2s / R = -4s cosθ\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e \u003cem\u003e/ l\u003c/em\u003e\u003c/p\u003e\u003cp\u003eWhere \u003cem\u003es\u003c/em\u003e is the surface tension, \u003cem\u003eR\u003c/em\u003e is the radius of the meniscus, \u003cem\u003eθ\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e is the contact angle on the surface, and \u003cem\u003el\u003c/em\u003e is the distance between two micropores. According to this formula, it can be known that when \u003cem\u003eθ\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e is less than 90\u0026deg; (the intrusion pressure \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e \u003cem\u003e\u0026lt;\u003c/em\u003e 0), the oil-water separation material can withstand a certain degree of liquid pressure. However, when \u003cem\u003eθ\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e is greater than 90\u0026deg; (the intrusion pressure \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003ei\u003c/em\u003e\u003c/sub\u003e \u003cem\u003e\u0026gt;\u003c/em\u003e 0), the liquid will gradually permeate through the oil-water separation material. Based on the above analysis, the contact angle of water on the surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM material in the air is 0\u0026deg;, so water can pass through CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM rapidly under the action of intrusion pressure. The contact angle of oil substances on the pre-wetted surface of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM all exceeds 150\u0026deg;, the material can repulse the penetration of oil substances. This theory further indicates that underwater superoleophobic CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM will possess great potential in the field of oil-water separation.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eUnderwater superhydrophobic materials have important application prospects in the field of efficient oil-water separation. Therefore, a self-made oil-water separation device was used to test the oil-water separation efficiency of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM material, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e11\u003c/span\u003e. Firstly, CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM was fixed in the oil-water separator and then pre-wetted with water. Secondly, the aqueous solution stained with methyl blue and corn oil were poured into the sand core funnel at a ratio of 1:1 (v/v). The methyl blue aqueous solution passed through CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM and flowed into the conical flask, while the corn oil was isolated at the top of the material. The reason for this phenomenon is that the underwater superoleophobic CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM with a dense micro-nano structure is pre-wetted to form a water film on its surface, which enables the oil phase to be isolated, while the water phase rapidly passes through the material under the action of gravity, achieving oil-water separation. Finally, the oil-water separation efficiency of the material can be calculated based on the volume of water before and after separation. Moreover, no obvious residual mixed liquid was observed in either the oil phase or the water phase after separation, which intuitively demonstrates the high oil-water separation efficiency of the material.\u003c/p\u003e\u003cp\u003eIn the practical application process, the separation efficiency of materials for different oil substances and the reusability of materials are both of crucial importance. Figure\u0026nbsp;12 shows that CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM can achieve the separation efficiencies of over 98% for four kinds of light oils (ethyl acetate, corn oil, liquid paraffin, and diesel oil) and two kinds of heavy oils (dichloromethane and glycerin). For the oil-water mixture with glycerol as the oil phase, the separation efficiency of the material can reach 99.5%. In addition, the reusability experiment of CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM was conducted using the glycerin-water mixture. After 60 cycles of oil-water separation, the used CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM still maintained stable oil-water separation efficiency of over 97% for glycerin. To sum up, the superhydrophilic and underwater superoleophobic CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM material prepared by simple and effective methods have great prospects for efficient oil-water separation.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e"},{"header":"4 Conclusions","content":"\u003cp\u003eIn conclusion, the underwater superoleophobic material based on SSM was successfully prepared by a facile and environmentally friendly in-situ flame method. By loading uniform and dense CaCO\u003csub\u003e3\u003c/sub\u003e-NCs onto the surface of the original substrate SSM, the material not only has superhydrophilicity in the air, but also the underwater contact angles of different oil substances all reach more than 150\u0026deg;, indicating that the material possesses underwater superoleophobic properties. This special wettability enables CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM to separate oil and water mixtures completely by gravity. The results of the sample performance test and characterization analysis show that the separation efficiency of this material for different oil substances can be maintained above 98%, and there is no obvious downward trend in its separation efficiency for glycerol after being reused 60 times. The micro-nano structure on the surface of the material enables it to form a water film underwater, thereby endowing the material with high self-cleaning property and anti-fouling performance. Therefore, this material holds great potential for the treatment of purifying oil-water mixtures and collecting oil pollutants from underwater environments.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis work was supported by Anhui Nature Science Research Program (Grant No. 2022AH051954), Huangshan University Science Research Program (Grant No. 2022xkjzd001), Youth Teacher Training Action Project of Anhui Province (DTR2023046).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor\u0026nbsp;contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAll authors have contributed to the research conception and design. The material preparation, data collection, and initial draft of the manuscript were carried out by Yinyu Sun and Caiyun Shen. The analysis of data and the drawing of charts were carried out by Wei Yang, Zihan Yin, Yu Liu, Qi Chen, Qing Ding, and Qiaoqiao Zhang. Changjiang Li and Zhongcheng Ke proofread the entire paper. All authors have provided comments on previous versions of the manuscript. All authors have read and approved the final manuscript.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflicts\u0026nbsp;of\u0026nbsp;interest\u0026nbsp;or\u0026nbsp;competing\u0026nbsp;interests\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe\u0026nbsp;authors\u0026nbsp;declare\u0026nbsp;that\u0026nbsp;they\u0026nbsp;have\u0026nbsp;no\u0026nbsp;known\u0026nbsp;competing\u0026nbsp;financial\u0026nbsp;interests\u0026nbsp;or\u0026nbsp;personal\u0026nbsp;relationships.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData\u0026nbsp;and\u0026nbsp;code\u0026nbsp;availability\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNot\u0026nbsp;Applicable\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eSupplementary information\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNot\u0026nbsp;Applicable\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eEthical approval\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNot Applicable\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eJ.F. 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Lange, Journal of Colloid and Interface Science. \u003cstrong\u003e298\u003c/strong\u003e, 899 (2006)\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"research-on-chemical-intermediates","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"rint","sideBox":"Learn more about [Research on Chemical Intermediates](http://link.springer.com/journal/11164)","snPcode":"11164","submissionUrl":"https://submission.nature.com/new-submission/11164/3","title":"Research on Chemical Intermediates","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"underwater superoleophobic, stainless steel mesh, CaCO3 nanoclusters, oil-water separation","lastPublishedDoi":"10.21203/rs.3.rs-6926943/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6926943/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eUnderwater superoleophobic materials have excellent underwater oil resistance due to their special wettability surface, which can cope with oil spill accidents and oily wastewater treatment. In recent years, metal-based underwater superoleophobic materials have attracted tremendous attention in the field of oil-water separation. However, the current methods for fabricating underwater superoleophobic materials have some shortcomings, such as complex preparation process, high cost, and secondary pollution. In this work, calcium carbonate nanoclusters (CaCO\u003csub\u003e3\u003c/sub\u003e-NCs), the product of thermal decomposition of calcium acetylacetone, were anchored on the surface of stainless steel mesh (SSM) by flame combustion method to fabricate an underwater superoleophobic material (CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM). The samples were characterized by field emission scanning electron microscope (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectrometer (XPS), and X-ray diffractometer (XRD). These results show that CaCO\u003csub\u003e3\u003c/sub\u003e-NCs can be uniformly and compactly anchored on the surface of SSM by flame combustion method. Moreover, the oil-water separation capacity and the reusability of the samples were also evaluated by a self-made oil-water separation device. CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM possesses excellent underwater superoleophobic property because of its uniform and dense hydrophilic micro-nano structure on the surface, which can absorb water to form a water film. It can also be known from the contact angle test that the underwater oil contact angles of ethyl acetate, corn oil, dichloromethane, glycerol, liquid paraffin, and diesel oil on the material surface are all greater than 150\u0026deg;. In the oil-water separation experiment, the separation efficiencies of this material for different oil substances all exceeded 98%, among which the separation efficiency of glycerin was 99.5%. In addition, CaCO\u003csub\u003e3\u003c/sub\u003e-NCs@SSM maintains a separation efficiency of more than 97% over 60 consecutive cycles of oil-water separation. In summary, the underwater superoleophobic material proposed in this paper has a facile preparation method and high oil-water separation efficiency, which has great potential in solving oil spill accidents and oily wastewater treatment problems in harsh environments.\u003c/p\u003e","manuscriptTitle":"Facile preparation of underwater superoleophobic stainless steel mesh for oil-water separation","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-07-14 08:36:33","doi":"10.21203/rs.3.rs-6926943/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-07-30T00:52:14+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-07-29T14:30:00+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-07-23T11:39:53+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"319503959622713039079421944958738483704","date":"2025-07-23T08:25:54+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"107923412050496101404206656993002228179","date":"2025-07-11T05:05:52+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-07-10T01:33:53+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-06-19T06:28:05+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-06-19T06:27:33+00:00","index":"","fulltext":""},{"type":"submitted","content":"Research on Chemical Intermediates","date":"2025-06-19T02:58:58+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"research-on-chemical-intermediates","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"rint","sideBox":"Learn more about [Research on Chemical Intermediates](http://link.springer.com/journal/11164)","snPcode":"11164","submissionUrl":"https://submission.nature.com/new-submission/11164/3","title":"Research on Chemical Intermediates","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"b568b9fe-c042-4b72-a4e1-4ee2463623d4","owner":[],"postedDate":"July 14th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2025-09-29T16:04:28+00:00","versionOfRecord":{"articleIdentity":"rs-6926943","link":"https://doi.org/10.1007/s11164-025-05757-4","journal":{"identity":"research-on-chemical-intermediates","isVorOnly":false,"title":"Research on Chemical Intermediates"},"publishedOn":"2025-09-26 15:58:15","publishedOnDateReadable":"September 26th, 2025"},"versionCreatedAt":"2025-07-14 08:36:33","video":"","vorDoi":"10.1007/s11164-025-05757-4","vorDoiUrl":"https://doi.org/10.1007/s11164-025-05757-4","workflowStages":[]},"version":"v1","identity":"rs-6926943","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6926943","identity":"rs-6926943","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}