Facile Synthesis of Smart Nanocontainers as Key Components for Construction of Self-Healing Coating with Superhydrophobic Surfaces
- Yi Liang†1,
- MingDong Wang†2,
- Cheng Wang†2,
- Jing Feng2,
- JianSheng Li1,
- LianJun Wang1 and
- JiaJun Fu1, 2Email author
© Liang et al. 2016
Received: 25 March 2016
Accepted: 19 April 2016
Published: 28 April 2016
SiO2-imidazoline nanocomposites (SiO2-IMI) owning high loading capacity of corrosion inhibitor, 1-hexadecyl-3-methylimidazolium bromide (HMID), and a special acid/alkali dual-stimuli-accelerated release property have been synthesized via a one-step modified Stöber method. SiO2-IMI were uniformly distributed into the hydrophobic SiO2 sol to construct “host”-“guest” feedback active coating with a superhydrophobic surface (SiO2-IMI@SHSC) on aluminium alloy, AA2024, by dip-coating technique. SiO2-IMI as “guest” components have good compatibility with “host” sol-gel coating, and more importantly, once localized corrosion occurs on the surface of AA2024, SiO2-IMI can simultaneously respond to the increase in environmental pH around corrosive micro-cathodic regions and decrease in pH near micro-anodic regions, promptly releasing HMID to form a compact molecular film on the damaged surface, inhibiting corrosion spread and executing a self-healing function. The scanning vibrating electrode technique (SVET) was applied to illustrate the suppression process of cathodic/anodic corrosion activities. Furthermore, benefiting from the superhydrophobic surface, SiO2-IMI@SHSC remained its protective ability after immersion in 0.5 M NaCl solution for 35 days, which is far superior to the conventional sol-gel coating with the same coating thickness. The facile fabrication method of SiO2-IMI simplifies the construction procedure of SiO2-IMI@SHSC, which have great potential to replace non-environmental chromate conversion coatings for practical use.
Chromate conversion coatings (CCCs) have been widely utilized as a pretreatment layer of protection of aluminium alloys due to their excellent barrier property and inherent self-healing feature . However, the high toxicity and carcinogenic effects of Cr(VI) substances deviate from the concept of sustainable environmental development, and the extremely strict regulations issued by the Environment Protection Agency of governments all over the world on CCCs require researchers to develop environmentally friendly alternatives with equal or better anticorrosion performance . Unfortunately, the protective abilities of various chemical conversion coating candidates, i.e. phosphate coating, rare earth conversion coating and permanganate/vanadate/tungstate conversion coatings, are still inferior to CCCs due to the lack of critical self-healing functionality. Self-healing coatings mimic the fundamental principle of living organisms, self-diagnose the internal defects or external mechanical damage and self-repair without any energy intervention to regenerate the integrity of coatings, which eliminate the potential risks, prolong the service life and achieve the long-term protection of underlying materials. Recently, Shchukin and Möhwald proposed the “host”-“guest” type of feedback active coatings (FACs), exhibiting the strong competitiveness and leading the research directions [3–7]. As a proof of conception, FACs are composed of two components: the “host” component (i.e. sol-gel coating and polymer coating) is responsible for the physical barrier, while the “guest” component, smart nanocontainers embedded in the “host” barrier coating provide an active self-healing nature. Once the aggressive species penetrate FACs through defects and initiate surface corrosion, smart nanocontainers can respond to the environmental changes around corrosive micro-regions, such as pH [8–13], electrochemical potential  and ionic strength [15, 16], and rapidly give the feedback, releasing entrapped corrosion inhibitors to depress corrosion spread. Organic corrosion inhibitors, including benzotriazole , 8-hydroxyquinoline  and benzimidazole , have been employed and successfully embedded into smart nanocontainers; once released, they can absorb on the metal surface and form a passive molecular film to retard the metal dissolution process by forming coordinate covalent bonds . From the point of view of working mechanisms, the key step in the fabrication of FACs is design and fabrication of smart nanocontainers, which should possess some important characteristics, including high loading capacity of corrosion inhibitors as healing agents, good compatibility with the “host” component and a stimuli-responsive-controlled release characteristic. In general, the construction of smart nanocontainers follows two steps: (i) the scaffolds are firstly rigorously screened, which determine loading efficiency and compatibility, (ii) in order to realize stimuli-responsive release, specially, to execute zero premature release under normal conditions and release corrosion inhibitors upon external stimuli deriving from corrosive micro-regions; various exquisite gatekeepers are installed on the surface of scaffolds through various methods, including polyelectrolyte layer-by-layer technique [21–23], supramolecular assembly  and organofunctionalization . Although FACs based on these smart nanocontainers demonstrate the outstanding corrosion resistance in experimental stage, the complicated routines for gatekeepers obstruct the up-scale production and the simple construction technique is attracting increasing attention and urgently needed [26–30].
Superhydrophobic surfaces, with static water contact angles higher than 150°, have attracted quite interest due to their unique water repellency and self-cleaning properties . Recently, many efforts have been made to fabricate superhydrophobic surfaces on aluminium alloy substrates, which serve as a barrier layer to prevent aggressive species from reaching the surfaces of the alloy substrates and exhibit the excellent anticorrosion performance [32–34]. Herein, in accordance with the sudden changes of pH occurring in corrosive micro-regions of aluminium alloy, we introduce a facile one-step method to fabricate the novel smart nanocontainers, SiO2-imidazoline nanocomposites (SiO2-IMI), based on the modified Stöber method. On balance, SiO2-IMI owning high loading capacity of corrosion inhibitor, 1-hexadecyl-3-methylimidazolium (HMID), good compatibility with “host” sol-gel coating and special acid/alkali dual-stimuli-accelerated release property, are regarded as the qualified candidates for smart nanocontainers. More importantly, the easy-to-accomplish procedure is expected to promote the industrialization of FACs. SiO2-IMI as smart nanocontainers were incorporated into the hydrophobic sol to construct “host”-“guest” FAC with a superhydrophobic surface (SiO2-IMI@SHSC). Through the evaluation of electrochemical impedance spectroscopy (EIS) and scanning vibrating electrode technique (SVET), the comprehensive anticorrosion performance, and the self-healing function of multifunctional coating, SiO2-IMI@SHSC were systematically evaluated.
Materials and Instrument
tetraethoxysilane (TEOS, ≥99.0 %), HMID and 1,1,1,3,3,3-hexamethyldisilazane (HMDS) were purchased from Sigma-Aldrich. N-propanol, methanol, ethanol, n-hexane, hydrochloric acid (HCl) and ammonia solution (conc. 28 %) were of analytical grade and used without further purification. Water was purified with a Millipore Q system and had an electrical resistance of 18 MΩ cm. Transmission electron microscopy (TEM; JEM-2100, JEOL) and field emission scanning electron microscopy (FESEM; S-4800, Hitachi) were used to examine the morphology of the SiO2-IMI and SiO2-IMI@SHSC. Fourier transform infrared (FTIR) spectra were recorded on a Bruker Tensor 27 FTIR spectrometer. Scanning transmission electron microscopy (STEM) imaging and EDX mapping were recorded from FEI-Tecnai G2 F30 S-TWIN TEM operated at 200 kV. Thermogravimetric (TG) analysis was performed using a Mettler TGA/SDTA 851e instrument with a heating rate of 10 K min−1 under nitrogen flow. UV/Vis spectroscopy was carried out with a Shimadzu UV-1800 spectrometer. An inductively coupled plasma optical emission spectrometer (ICP-OES; PerkinElmer Optima 4300 DV) was used to monitor the amount of Si in a supernatant. The static contact angle (CA) was measured by a CA meter (XG-CAMB, XuanYi Instrument Ltd., China). The X-ray photoelectron spectra (XPS) of the coating were collected on a PHI QUANTERA II X-ray photoelectron spectrometer, using a monochromatic Al Kα radiation (λ = 8.4 Ǻ) as the exciting source. Atomic force microscopy (AFM; Vecco Brook DI) was used to characterize the topography of the surface of coated aluminium alloy specimens and operated in tapping mode. Raman spectroscopy was conducted using a laser confocal inVia Raman microspectrometer (Renishaw, UK) equipped with a 514-nm Ar ion solid excitation laser. Electrochemical measurements were carried out with a PARSTAT 2273 potentiostat/galvanostat (Princeton Applied Research, USA). SVET measurements were performed on equipment from Applicable Electronics Inc. (USA).
Preparation of SiO2-IMI
A simple procedure described below was followed for the modified Stöber method . In a typical synthesis, 10 mg HMID was added to a mixture of 80 mL ethanol with 3.0 mL ammonia solution (conc. 28 %). After stirring for 30 min, 0.1 mL TEOS was added dropwise to the solution. The molar ratio for TEOS:HMID:NH3·H2O was controlled as 17.3:1:929. The mixture was left to react under stirring at room temperature for another 24 h. The SiO2-IMI nanoparticles were collected by centrifugation, washed with ethanol and dried under vacuum overnight for further use.
Preparation of SiO2-IMI@SHSC
The typical preparation route of SiO2-IMI@SHSC includes four steps: (1) formation of SiO2 gel; (2) modification of the surface of SiO2 gel with HMDS through covalently bonding with interfacial reactive –OH group to form hydrophobic SiO2 gel; (3) transformation of hydrophobic SiO2 gel to hydrophobic SiO2 sol with the aid of ultrasonication; (4) incorporation of SiO2-IMI into hydrophobic SiO2 sol and then to produce the novel type of “host”-“guest” FAC with a superhydrophobic surface, SiO2-IMI@SHSC (Fig. 4A), on AA2024 by dip-coating technique. Typically, 5.35 mL TEOS was first dissolved in 10 mL methanol, and then a mixture of 7.5 mL NH4OH (0.02 N) and 10 mL methanol was added to the solution. After stirring at room temperature for 2 h, 3.65 mL HCl (0.1 N) was added to the mixture. For adjusting the pH of the mixture close to 8.0, the appropriate amount of NH4OH solution was added. The SiO2 gel was formed after ageing for 20 h. Thereafter, 5 mL HMDS in 47 mL n-hexane was added to the SiO2 gel. After keeping at 60 °C for another 20 h in a closed container, the hydrophobic SiO2 gel was obtained. After that, the hydrophobic SiO2 gel was dispersed in 40 mL n-propanol by ultrasonication and centrifuged with a speed of 1000 rpm for 15 min to transform to the hydrophobic SiO2 sol. Then, SiO2(0.1 g) was added into 9.9 g the hydrophobic SiO2 sol for 5 min stirring to form a composite sol for the next dip-coating procedure.
SiO2-IMI@SHSC coating was prepared on an aluminium alloy surface (AA2024, 40 mm × 20 mm × 2 mm) the by dip-coating procedure. The pretreated AA2024 specimen was immersed into the composite sol for 5 min followed by withdrawal at a speed of 10 mm min−1 to complete the first round. The process was repeated for another three times using pure hydrophobic sol (no SiO2-IMI addition). The coating sample was air-dried at 120 °C for 2 h.
Acid/Alkali Dual-Stimuli-Accelerated Release Experiments
In order to investigate the acid/alkali dual-stimuli-accelerated release characteristic of SiO2-IMI, UV/Vis spectroscopy was used to determine the concentration of HMID released from SiO2-IMI in a supernatant using the standard curve (Additional file 1: Figure S1). Briefly, SiO2-IMI (1 mg) were placed in the dialysis membrane at the top of the quartz cuvette to avoid interference. The solution (4 mL) of different pH values (neutral, PBS buffer solution 7.0; acidic, adjusted by HCl solution; alkaline, adjusted by NaOH solution) was carefully added into the cuvette to ensure that SiO2-IMI were completely immersed into the solution. Release profiles were obtained by plotting the absorption of HMID in the supernatant at λ = 210 nm as a function of time. In the first 4 h, the real-time monitoring of HMID was recorded at 1-s intervals.
A conventional three-electrode electrochemical cell was used, which consists of a working electrode, a saturated calomel electrode (SCE), as a reference electrode and a platinum sheet as a counter electrode. Electrochemical impedance spectroscopy (EIS) measurements were performed using a PARSTAT 2273 potentiostat/galvanostat in a frequency range from 100 kHz down to 10 mHz. The coated AA2024 specimens were used as a working electrode, and the exposed area was approximately 1.0 cm2. The EIS measurements were carried out at an open-circuit potential (OCP) using a sine wave of 10 mV amplitude peak to peak. The impedance data were fitted to appropriate equivalent circuits by using ZSimpWin software. For the Tafel polarization measurements, the AA2024 specimens or the coated AA2024 specimens were used as the working electrode, and the exposure area was about 0.5 cm2. The Tafel plots were obtained by changing the electrode potential automatically from −250 mV to +250 mV at the OCP at a scan rate of 0.166 mV s−1.
SVET measurements were conducted on a commercial system from Applicable Electronics controlled by ASET software. The vibrating microelectrode is a Pt-Ir microprobe with a Pt black tip (15-μm diameter), which was moved at a distance of 200 μm above the exposed surface of the tested specimens on a lattice of 21 × 21 points over an area of 4 × 4 mm2 (step size 200 μm). The current densities are presented in the form of 3D maps. Scans were started after 1 h immersion and were automatically collected every 2 h for the duration of the experiments. All the tests were conducted at the OCP.
Results and Discussion
Characterization of SiO2-IMI
Acid/Alkali Dual-Stimuli-Accelerated Release of HMID from SiO2-IMI
Amount of Si in the supernatant during release experiments
Amount of Si (mg/L)
Based on the Stöber method, SiO2-IMI was successfully synthesized by introducing appropriate amounts of HMID at the beginning stage of reaction and precisely controlling reaction conditions. During the process of ammonia-catalysed hydrolysis and condensation of TEOS, the silica species carry high negatively charged density under alkaline condition and are apt to bind with positively charged HMID molecules via strong electrostatic attraction. Due to the high initial concentration of HMID, the composite condensation product quickly exceeds the critical saturation, and a large amount of stable silica-HMID nuclei are formed and further aggregated. As the reaction proceeded, the massive consumption makes the shortage of HMID in the later SiO2-IMI growth stage. The specific “interior-rich and exterior-deficient” distribution framework for HMID dominates the acid/alkali dual-stimuli-accelerated release. SiO2-IMI showed the good stability in neutral solution within a certain time; however, the slight degradation phenomenon appeared for longer time observation, which also had been reported in some previous literatures . The experimental data verify that the presence of H+ and OH− evidently accelerate the self-degradation rate. Combined with the representative TEM images, the persistent infiltration of H+ and OH− through open pores stemming from particles packing undoubtedly destroyed the original charge balance of silica-HMID nuclei, the abrupt disappearance of strong electrostatic attraction resulted in the fact that the more aggregations of silica-HMID nuclei dissociated from SiO2-IMI and dispersed in the supernatant [39, 40]. The nonuniform distribution of silica-HMID nuclei determines disintegration mode of “from interior to exterior” . Under a H+ or OH− attack, the central interior regions completely collapsed and the hollow structure emerged. The outmost layer of SiO2-IMI retained the intact state due to its stable silica constituents and lack of silica-HMID nuclei, confirming our hypothesis for growth mechanism of SiO2-IMI. In addition, the morphology of SiO2-IMI after 4 days of immersion under pH 4.0 changed greatly (Fig. 3b (e)). The fast dissolution of silica-HMID nuclei within the interior regions may result in the irregular morphology. The acid/alkali stimuli-accelerated release mode is depicted in Fig. 3c.
Construction of Multifunctional Coating, SiO2-IMI@SHSC
Comprehensive Anticorrosion Performance Evaluated by EIS
Self-Healing Function Evaluated by SVET
In summary, a facile approach to acid/alkali dual-stimuli-accelerated release system, SiO2-IMI, was demonstrated. Considering the high content of corrosion inhibitors, SiO2-IMI have the potential to be ideal smart nanocontainers for “host”-“guest” FACs to execute self-healing tasks in the corrosive micro-regions upon pH stimuli. The sol-gel coating with superhydrophobic surfaces was constructed as a “host” barrier coating component, and the good compatibility between the “host” coating and “guest” SiO2-IMI makes the fabricated multifunctional coating, SiO2-IMI@SHSC, work normally. SiO2-IMI@SHSC exhibited the excellent long-term anticorrosion performance in 0.5 M NaCl depending on the superhydrophobic, water-repellent surface and active corrosion protection from the incorporated SiO2-IMI. When SiO2-IMI@SHSC was mechanically scratched, SiO2-IMI were in response to corrosive environmental stimuli and released embedded HMID molecules to form protective molecular film and provide the reliable protection for a damaged metal surface. The outstanding comprehensive anticorrosion capacity and the simple preparation technique will make the multifunctional coating become a promising candidate to replace non-environmental chromate conversion coatings for the protection of aluminium alloys.
The authors thank Shanghai Equshine Scientific Instruments Co. Ltd. for providing the SVET measurements. The authors thank the Fundamental Research Funds for the Central Universities, No 30915011312 and No 30915012207; the QingLan Project, Jiangsu Province, China; a Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD); the Industrial Research Project, No CG1421; Science and Technology Bureau of Lianyungang City; and the Prospective Joint Research Project, No BY2015050-01, Jiangsu Province, China.
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