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Wetting Properties and Thin-Film Quality in the Wet Deposition of Zeolites Yi-Chen Huang,† Wan-Ju Hsu,† Cheng-Yang Wang,‡ Heng-Kwong Tsao,‡ Yu-Hao Kang,§ Jiun-Jen Chen,*,§ and Dun-Yen Kang*,† †
Department of Chemical Engineering, National Taiwan University, Taipei 10617, Taiwan, ROC Department of Chemical and Materials Engineering, National Central University, Taoyuan 32001, Taiwan, ROC § Green Energy and Environment Research Laboratories, Industrial Technology Research Institute, Hsinchu 31040, Taiwan, ROC Downloaded via 31.40.211.143 on August 15, 2019 at 07:53:16 (UTC). See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.
‡
S Supporting Information *
ABSTRACT: Zeolites are microporous crystalline materials widely used in catalysis and adsorption applications. The fabrication of zeolite thin films and membranes has also opened up the possibility of using zeolites in electronic devices and membrane separations. The existing approach to growing zeolite films involves exposing the substrate to a high-pH environment; however, this process is applicable to only specific types of substrates. Our group has developed the direct wet deposition of zeolites via ultrasonic nozzle spray deposition to address this issue; however, the relationship between wetting properties and thin-film quality has yet to be investigated. In this study, we prepared zeolite CHA (Si:Al:P = 3:10:20) suspensions using different solvents and surfactants in various concentrations. We then examined the relationships among the composition of the cast solution, their wetting behavior on the glass substrate, and the uniformity of the resulting thin films. We found that using ethanol as a solvent with zeolite crystals in low concentrations with added surfactant yielded zeolite films of high quality. We were also able to produce low-haze zeolite coatings on glass. The zeolite coatings with high hydrophilicity and adsorption capacity presented excellent antifogging capability.
1. INTRODUCTION Zeolites are crystalline microporous aluminosilicates with a well-defined pore topology and high thermal and mechanical stability. Zeolites in a powder or pellet form have been broadly used in catalysis,1−4 adsorption,5,6 and ion exchange.7,8 Developments in zeolite thin films and membranes have also enabled the application of zeolites in membrane-based separation9−11 and thin film-based electronics.12−16 The methods used in the fabrication of zeolite films/membranes can be categorized into two classes. The first class requires the formation of zeolite films/membranes during the crystallization of zeolites, which involves in situ crystallization,17−19 seeded growth,20,21 and dry gel conversion.22,23 The second class requires a zeolite suspension with fully grown crystals, which involves dip coating,24,25 spin-on deposition,26−29 or spray deposition.14,30 The second class avoids the need to expose the substrate to a high-pH environment during zeolite crystal growth, thereby making it possible to deposit zeolites on silicon wafers,29,31,32 glass substrates,33,34 and aluminum alloy.35,36 Ultrasonic nozzle spray deposition (UNSD) is a relatively new technique wherein ultrasonic vibrations are used to create a high-frequency standing wave, which generates uniform © XXXX American Chemical Society
droplets in the tens of micrometers. The droplets formed from cast solution deposited on the substrate form a homogenous film.37−41 UNSD has been used for the deposition of polymers42−46 and small organic molecules.47,48 Only a few reports have addressed the use of UNSD in the preparation of zeolite films.14 Several factors can affect the quality of zeolite films prepared using UNSD, including the operating conditions for spraying, the composition of the cast solution, and the wetting behavior of the solution on the substrate. Our group has optimized the quality of zeolite films by varying the operating conditions and composition of the cast solutions.14 However, the effects of wetting behavior of the cast solution on deposition quality have yet to be reported. In this paper, we examine the relationship between the wetting properties of zeolite suspensions on a glass substrate and thin-film quality using the zeolite CHA (Si:Al:P = 3:10:20). Water and ethanol were used as solvents for suspending zeolites. Spreading dynamics and contact angle measurements were applied to investigate wetting behavior. Received: June 17, 2019 Accepted: July 16, 2019
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15% were used in the UNSD on 25 × 25 mm glass substrates. The UNSD device in this study (model: USD-1515) was purchased from Nano Optical Coating Technology Inc. This system is equipped with an ultrasonic atomizer nozzle operating at a frequency of 60 kHz with tunable piezo power between 0.5 and 5.0 W. Nitrogen was used as the carrier gas at a pressure of 10 psi during the coating process. The nozzle-tosubstrate distance was fixed at 60 mm, and the injection flow rate of the cast solution was maintained at 1 mL/min. The moving pathway of the nozzle across the substrates is illustrated in Figure S1. The moving speed of the nozzle along the y-axis was maintained at 200 mm/s, and moving speed along the x-axis was maintained at 100 mm/s. After UNSD, the coated substrates were placed in an oven and baked at 100 °C for 1 h. Thin-film samples were then transferred to a furnace for calcination. The temperature in the furnace was increased from room temperature to 550 °C (at a heating ramp rate of 1 °C/min), where it was held for 6 h. Following calcination, the thin-film samples were ready for material characterization. 2.6. Material Characterization. The micromorphology of the thin-film samples was analyzed using optical microscopy (OM, Whited WM-100) and scanning electron microscopy (SEM, Hitachi S4800). SEM was operated at an acceleration voltage of 10 kV. A thin layer of gold was deposited on the samples prior to SEM characterization. Grazing-incidence X-ray diffraction (XRD) for the thin films was performed using a PANalytical X’Pert diffractometer with a Cu Kα source operated at a voltage of 45 kV and an incident angle of 1°, scanning from 5° to 35° 2θ with a step size of 0.02°. The haze of the various thin-film samples was measured according to ASTM Method D1003 using an Agilent Cary 300 UV−vis spectrophotometer. The measurements were obtained using a double beam with a spectral bandwidth of 2.0 nm at a scanning rate of 600 nm/min. The wettability of the thin-film samples was determined according to contact angles recorded using a DataPhysics (Krü ss, Germany) DSA25E contact angle measurement system. This involved releasing a water droplet of 5 μL from a micropipette onto the thin-film surface and monitoring the evolution of the droplet. Antifogging properties were evaluated by placing thin-film samples over a glass of boiling water (approximately 40 mL). Photographic images were recorded after the samples had been exposed to water vapor for 30 s. The samples were then dried using a high-pressure nitrogen gun and stored under ambient conditions for 24 h prior to the next test. The antifogging test was repeated seven times for evaluating the durability of the zeolite films.
Optical microscopy, scanning electron microscopy, and UV− visible spectroscopy were used to characterize the deposition quality on the glass substrates. We also assessed the antifogging capability of uniform zeolite CHA films cast on glass substrates.
2. EXPERIMENTAL DESIGN 2.1. Chemicals. Aluminum isopropoxide (98+%) and tetraethylammonium hydroxide (TEAOH) solution (35 wt % in water) were purchased from Alfa Aesar. Tetraethyl orthosilicate (TEOS, 99%) and ethanol (99.9%) were purchased from Merck. Phosphoric acid (85 wt % in water) and TWEEN 80 were purchased from Sigma-Aldrich. All chemicals were used without further purification. The deionized (DI) water used in the synthesis process was obtained using the ELGA PURELAB Classic DI ultrapure water system. 2.2. Preparation of Zeolite CHA Suspensions. The synthesis method used in this study followed our previous report with minor modifications.49 We added 2.0 g of aluminum isopropoxide to 8.25 g of TEAOH solution. The mixture was placed in a perfluoroalkoxy alkane container with a maximum capacity of 100 mL and stirred at 30 °C for approximately 1 h until the solution became completely transparent. We then added 0.61 g of TEOS to the solution and stirred it for 2 h, before adding 2.26 g of phosphoric acid to obtain a final molar ratio of 1 Al(OPri)3:2 H3PO4:0.3 SiO2:2 TEAOH:30 H2O with a total mass of 13.1 g. The mixture was aged at room temperature for 1 h under agitation and then transferred to a Teflon-lined autoclave (maximum capacity of 180 mL) to undergo a hydrothermal reaction in a convection oven at 180 °C over a period of 8 h. Following the hydrothermal synthesis, the suspension was then centrifuged at 20 000 rpm for 30 min using HERMLE Centrifuge Z 36 HK. The resulting supernatant was decanted, and fresh water was added to the precipitate until it reached the original mass. The centrifugation process was repeated three times. After the last centrifugation, DI water or ethanol was added to the precipitate comprising crystals of the zeolite CHA, until it reached the original mass (approximately 12 g). The water suspension was diluted by six times (denoted as W-6×) to form a cast solution. The ethanol suspension was subjected to various dilutions. The suspension diluted by three times was denoted as E-3×, and the remaining samples were named by analogy. TWEEN 80 was added to some of the cast suspensions. E-6× with 2.5 mass percent of TWEEN 80 was denoted as E-2.5%, and the remaining samples were named by analogy. All of the cast solutions were stirred at room temperature prior to thin-film deposition via UNSD. 2.3. Substrates for Thin-Film Deposition. Corning EAGLE XG alkali-free glass with a thickness of 0.7 mm was cut into squares (approximately 25 × 25 mm) prior to UNSD. 2.4. Characterization of Suspensions. The equilibrium contact angle and the surface tension of the zeolite CHA suspensions were measured using a DataPhysics DSA25E (Krüss, Germany) contact angle measurement system. This involved releasing a 5 μL droplet of the suspension from a micropipette onto the surface of the glass substrate. The topview shape evolution of a suspension droplet on the glass substrate was recorded using a charge-coupled device camera from which the spreading area was analyzed using ImageJ.50 2.5. Preparation of Zeolite CHA Thin Films. Zeolite CHA suspensions W-6×, E-3×, E-6×, E-10×, E-2.5%, and E-
3. RESULTS AND DISCUSSION 3.1. Effects of Solvents. Figure S2 presents photographic images of the zeolite suspension in water (W-6×) and ethanol (E-6×). We did not observe pronounced precipitation in either suspension after standing for 24 h, indicating that the suspensions were highly stable. Nonetheless, the deposition of W-6× and E-6× on the glass substrate resulted in samples with remarkably different surface morphologies, as shown in Figure 1. The W-6× presented poor wetting behavior on the glass substrate prior to baking, which resulted in a highly nonuniform surface after baking. In contrast, the E-6× presented good wetting behavior, which resulted in a highly B
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6× permitted complete wetting51 on the substrate, which resulted in a uniform surface morphology of the deposition. The slow evaporation of water may also explain the poor uniformity of thin films prepared using W-6×.52,53 There was almost no difference between E-6× and pure ethanol in terms of contact angle and surface tension; however, there was a notable difference between W-6× and pure water. Such dewetting behavior can be attributed to the particle−fluid interaction in W-6× and the long-range electrostatic interactions among zeolite particles.54,55 The surface tension of W-6× was slightly lower than that of pure water, probably due to the presence of zeolite particles creating density fluctuations in the suspension, which destabilized the droplets.56 The above results suggest that ethanol is superior to water as a solvent for the deposition of zeolite CHA. Thus, we limited subsequent analysis to samples prepared using ethanol. We investigated the degree to which the concentration of zeolite particles in the suspensions affects deposition quality. E6× suspension was concentrated by two times to produce E3×, and diluted by 1.67 times to produce E-10×. The SEM images of the thin films formed by the three suspensions are presented in Figure 3. Ring patterns at the scale of tens of micrometers were observed in E-3× and E-6×. It is likely that these patterns are examples of the coffee-ring effect, in which colloidal particles are carried radially outward via capillary flow during the evaporation of the solvent.57−59 The ring patterns Figure 1. Photographic images of zeolite suspensisons deposited on the substrate before (1st row) and after (2nd row) baking, and topview OM images (3rd row) of zeolite CHA thin films prepared using (a) W-6× and (b) E-6×.
homogeneous thin film on the substrate. This is a clear indication that the solvent plays a key role in the wet deposition of zeolites. Suspensions (W-6× and E-6×) and pure solvents were measured in terms of contact angle and surface tension (Figure 2). The contact angle of W-6× (37.5°) was relatively higher than that of E-6× (as low as 0°). The surface tension of W-6× (74.4 mN/m) was approximately three times higher than that of E-6× (23.3 mN/m). The high surface tension of W-6× resulted in droplets with a high contact angle in order to minimize the free energy of the system, resulting in poor wetting on the glass. In contrast, the low surface tension of E-
Figure 2. Equilibrium contact angles on the glass substrate and surface tensions of water, ethanol, and various zeolite CHA suspensions.
Figure 3. Top-view SEM images of zeolite CHA thin films cast from suspensions of (a) E-3×, (b) E-6×, and (c) E-10×. C
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were less noticeable in E-10× than in E-3× and E-6×, which suggests that the dilution of the zeolite CHA suspensions facilitated the merging of droplets during solvent evaporation, thereby suppressing the coffee-ring effect. We studied the spreading dynamics of the three suspensions and pure ethanol in order to gain insight into the effects on deposition quality. Figure 4 presents results of droplet
Figure 4. (a) Temporal evolution of droplets of various zeolite CHA suspensions spreading on the glass substrate; (b) log−log plot showing spreading area vs time. Figure 5. Photographic images (1st row), top-view OM images (2nd row), and SEM images (3rd and 4th row) of zeolite CHA thin films prepared using (a) E-2.5% and (b) E-15%.
spreading area versus time. We found that the maximum droplet spreading area decreased with an increase in the concentration of colloidal particles. The small maximum spreading area of E-3× suggests that the solvent may have fully evaporated before droplets merged with adjacent droplets. This finding is in good agreement with the pronounced coffeering effects observed in E-3×. The droplet-spreading rate can be quantified using the slope in a log−log plot (Figure 4b).60,61 The slope of pure ethanol, E-10×, and E-6× was approximately 0.60, whereas the slope of E-3× was 0.51. The relatively slow spreading of E-3× can be attributed to the high viscosity caused by the high concentration of colloidal zeolite particles.62 3.2. Effects of Surfactants. Nonionic surfactants, such as TWEEN 80, are widely used to stabilize the cast solutions used in the deposition of zeolite thin films.16,49,63,64 In this study, we used TWEEN 80 to minimize the coffee-ring effects during the deposition of the zeolite CHA films. The zeolite suspension in ethanol (E-6×) with TWEEN 80 added at wt % of 2.5 and 15 are, respectively, denoted as E-2.5% and E-15%. Figure S3 presents photographic images of suspensions with various TWEEN 80 contents. We found that E-2.5% and E-15% were both highly stable. Figure 5 presents photographic, OM, and SEM images of thin films deposited using these two suspensions. Samples E-2.5% and E-15% did not present ring patterns, probably due to the addition of TWEEN 80 prior to
wet deposition. According to previous reports,63,65,66 the minimization of coffee-ring effects can be attributed to an increase in viscosity following the addition of surfactants. The SEM images revealed a larger number of void spots in E-15% than in E-2.5%. This can be attributed to the fact that micelles formed by the surfactant increased interparticle spacing during deposition, which ultimately resulted in void spots after calcination.67 The contact angles of E-2.5%, E-15%, and pure ethanol were all close to zero; however, the surface tension of E-2.5% and E-15% was slightly lower than that of pure ethanol (Figure S4). We examined the spreading dynamics of E-2.5% and E-15% to gain insight into the differences in deposition quality (Figure 6). E-2.5% and E-15% both showed faster spreading dynamics (i.e., larger slope in the log−log plot) than did the suspensions in the absence of surfactants (E-3×, E-6×, and E-10×). This can be attributed to two factors. First, the surfactant reduced the overall surface tension of the solution.68 Second, the presence of surfactants resulted in a more homogeneous distribution of zeolite colloids throughout the suspension.69 Despite a similar spreading rate, the spreading area of E-2.5% exceeded that of E-15%. This can be attributed to the fact that D
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Figure 6. (a) Temporal evolution of droplets of various zeolite CHA suspensions spreading on glass substrate; (b) log−log plot of spreading area vs time.
Figure 7. (a) Photographic images of various zeolite CHA thin films 7.5 cm from letters beneath; (b) haze measurements of various zeolite CHA thin films.
a higher concentration of TWEEN 80 resulted in higher viscosity, which hindered the spreading of the suspension. Nevertheless, the addition of surfactants to zeolite cast solutions greatly enhances the spreading rate and suppressed the coffee-ring effect, which helped to create a highly uniform coating. 3.3. Antifogging Properties. The coatings with relatively high quality (E-6×, E-2.5%, and E-15%) were subjected to antifogging tests. One requirement of an antifogging film is low-transmission haze. The haze of the three samples was qualitatively analyzed using photographic images (Figure 7a). Samples E-2.5% and E-15% presented less haze than did E-6×. Quantitative analysis of transmission haze was conducted using UV−vis spectroscopy. The spectral average values are summarized in Figure 7b. The quantity of transmission haze presented by E-2.5% and E-15% was close to that of bare glass. In contrast, E-6× presented remarkably higher transmission haze than did the other samples. High-transmission haze is usually caused by pronounced light scattering.70−72 The micrometer ring patterns in sample E-6× caused strong light scattering. E-15% possessed slightly higher haze than did E2.5%. This may be due to light scattering is induced by an excessive number of void spots, as shown in the SEM images in Figure 5. The thickness of thin film E-6×, E-2.5%, and E-15% was determined using the cross-sectional SEM images (Figure S5), which suggests a thickness of approximately 900 nm for these three samples. Antifogging tests were conducted on a bare glass substrate as well as the zeolite thin-film samples. The tests involved exposing samples to hot water vapor for a period of 30 s, and a
photo was recorded for assessment of the antifogging property. The samples were stored under ambient conditions for 24 h between each test. Seven tests were conducted on each sample. The results of the 1st, 5th, and 7th tests (E-6×, E-2.5%, and E15%) are summarized in Figure 8a. All three samples showed good antifogging capability in comparison to the bare glass, and E-15% presented the best results. More specifically, trace numbers of small droplets formed on E-6× and E-2.5%, whereas no droplets were observed on E-15% during the tests. The results are in good agreement with the wettability analysis of zeolite CHA thin films (Figure S6), which showed that sample E-15% possessed a lower water contact angles than E6× and E-2.5% did. This suggests that the high surface hydrophilicity of E-15% may explain its good antifogging performance. XRD analysis (Figure 8b) was used to gain insight into the differences in antifogging capability. All of the samples possessed high crystallinity of the zeolite CHA phase; however, the ratio of the amorphous phase in sample E-15% was higher (a higher intensity hump between 17 and 30° 2θ) than that of the other two samples. In our previous research,33 we determined that a high ratio of amorphous phase can have a negative effect on antifogging performance; however, our findings in this study contradict those results. It is possible that these voids assist in the diffusion of water vapor in zeolite films, thereby improving the overall efficiency of the zeolite layer in the adsorption of water molecules. The unique microstructure of E-15% may play a key role of its antifogging performance. E
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related to the degree of thin-film crystallinity. Specifically, the well-defined pore topology of the highly crystalline zeolite films was shown to assist in the adsorption of water vapor, thereby improving antifogging performance. In summary we identified the key parameters affecting the uniformity and antifogging capability of the zeolite thin films prepared using the direct wet deposition, and the information presented in this work could be used to extend the fabrication of zeolite thin films to a variety of substrates for a range of applications.
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ASSOCIATED CONTENT
S Supporting Information *
The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acsomega.9b01794. Schematic illustration showing movement pathway of ultrasonic nozzle across glass substrate, photographic images of zeolite CHA suspensions, equilibrium contact angles of various zeolite CHA suspensions on the substrate, cross-sectional SEM images, wettability analysis of water droplet on CHA thin films, and the photographic images of E-15% subject to a treatment in a sonication bath (PDF)
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AUTHOR INFORMATION
Corresponding Authors
*E-mail:
[email protected] (J.-J.C.). *E-mail:
[email protected] (D.-Y.K.). ORCID
Heng-Kwong Tsao: 0000-0001-6415-8657 Dun-Yen Kang: 0000-0002-2349-4432
Figure 8. (a) Antifogging test of thin films following daily exposure to hot water vapor for 30 s; (b) XRD patterns of various zeolite CHA thin films.
Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS This work was supported by the Bureau of Energy of the Ministry of Economic Affairs of Taiwan. The authors would like to thank Chin-Yan Lin and Ya-Yun Yang at the Electron Microscope Unit of the Instrument Center at National Taiwan University for their valuable assistance in obtaining SEM images.
We placed the best-performed sample, E-15%, in an ultrasonic bath for 30 and 60 s, and partial peel-off was observed (Figure S7). The improvement of the adhesion between the zeolites and the glass substrates is necessary before the commercialization of the antifogging coating present in this work.
4. CONCLUSIONS In this study, we investigated the relationships among the composition of zeolite suspensions, wetting behavior of the suspensions on the substrate, and the quality of zeolite CHA thin films (Si:Al:P = 3:10:20) deposited using UNSD. We found that ethanol was superior to water when used as a solvent for the dispersion of zeolite crystals. Zeolite suspended in ethanol produced thin films of relatively high uniformity on glass substrates when applied using UNSD. This can be attributed to the good wetting behavior of ethanol on glass substrates as well as its rapid evaporation. Reducing the concentration of zeolite crystals in the cast solution or adding surfactant (TWEEN 80) was shown to eliminate nonuniform patterns in the thin films. Both of these approaches were shown to enhance the spreading dynamics of the zeolite colloidal solutions on the glass substrate. In our analysis, we observed a positive correlation between spreading dynamics and thin-film quality. The zeolite CHA crystals deposited on the glass substrate using UNSD under the optimized conditions presented low haze and good antifogging properties. We also found that the antifogging performance was
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REFERENCES
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DOI: 10.1021/acsomega.9b01794 ACS Omega XXXX, XXX, XXX−XXX
