Journal of Materials Science

, Volume 55, Issue 2, pp 498–508 | Cite as

Superhydrophilic–superhydrophobic patterned surfaces on glass substrate for water harvesting

  • Jichao Zhang
  • Faze Chen
  • Yao Lu
  • Zhongtao Zhang
  • Jiyu Liu
  • Yang Chen
  • Xin LiuEmail author
  • Xiaolong YangEmail author
  • Claire J. Carmalt
  • Ivan P. Parkin


Directional water harvesting is a special ability of flora and fauna in nature. Wettability-patterned surfaces inspired by natural structures have been extensively researched and could be a great potential avenue for easing water shortage. However, preparation strategies for these nature-inspired cases, including UV irradiation with mask technology, femtosecond laser direct writing and chemical treatment, are time-consuming, cost-ineffective and environmentally unfriendly. In this paper, robust and durable superhydrophobic (SHB) glass substrate was prepared by using laser-induced backward transfer technique and fluoroalkylsilane modification. Then wedge-shaped superhydrophilic (SHL) patterns on the SHB surfaces were rapidly constructed by inexpensive and commercially available fibre laser ablation for fog harvesting. This facile, cost-effective and non-corrosive preparation method described herein could be an alternative way to construct SHL–SHB patterns on glass substrate, which could be used for microfluidic devices, droplet manipulation and cell screening.


Water harvesting is a special ability of flora and fauna in nature [1, 2]. For example, Namib Desert beetles could live in arid environment due to water harvesting on their back exoskeleton where waxy hydrophobic and non-waxy hydrophilic regions are alternately distributed [3]. Various extremely drought-tolerant plants like cactaceae species could survive in the desert with great fog harvesting performance via well-distributed conical spines and trichomes on their surfaces [4, 5, 6, 7]. Likewise, spider silk also possesses excellent water harvesting ability because of unique fibre structures of spindle knots and joints [8, 9, 10]. These natural cases inspired research focusing on construction of wettability-patterned surfaces or special structures to collect water, which shows great potential to alleviate water scarcity in terms of regional water shortage [11].

Wettability-patterned surfaces have been extensively created by mask-based methods. For example, Lin et al. [12] deposited copper on a polyethylene terephthalate (PET) surface via mask-assisted sputtering and then obtained superhydrophilic (SHL) wedge-shaped tracks on the PET substrates by alkali-assisted copper oxidation. The as-prepared patterned surface showed high water harvesting efficiency. Song et al. [13] proposed a mask-assisted chemical etching method to create superhydrophobic (SHB)–SHL patterns on various metal substrates for fog harvesting. Yang et al. [14] described a double electrochemical etching and boiling water immersion method to fabricate SHL–SHB wedge-shaped pattern on Al substrate with the assistance of masks for fog harvesting. The aforementioned works demonstrated enhanced water harvesting performance of wettability-patterned surface, but these reported methods involve the use of masks and corrosive chemical solutions, suffering from low processing efficiency and large environmental impact.

Glass substrates are widely used in various fields, such as houses and automobiles, where frequent fog condensate could be observed. Therefore, it should be of great importance to create extreme wettability patterns on glass surface to improve its water harvesting performance. Several methods, including hydrofluoric acid etching [15, 16] and laser direct writing (LDW) [17, 18, 19, 20, 21, 22, 23], have been proposed to texture glass substrates. LDW is considered as a rapid, green and highly efficient non-contact machining method. Laser-induced backward transfer (LIBT) is a LDW technology that could realize material deposition on transparent receiver substrates from donor substrates [24, 25, 26, 27]; thus, it could be an alternative tool to create special surface structures on glass substrate for further wettability control. However, to the best of our knowledge, LIBT has been rarely employed to impart glass substrate superwettability.

In this paper, we firstly obtained robust and durable superhydrophobic glass substrate by using LIBT technique and fluoroalkylsilane (FAS) modification. Then wedge-shaped superhydrophilic patterns on the superhydrophobic surfaces were rapidly constructed by laser ablation. The as-prepared SHL–SHB patterned surface shows impressive fog harvesting ability with an efficiency of 15.68 mg cm−2 min−1. Compared to the reported previous studies, our work possesses a high water collection efficiency with this facile, cost-effective and non-corrosive preparation method.

Experimental section

Fabrication of SHL–SHB patterns on glass substrate

As illustrated in Fig. 1, deionized water cleaned slide glass (70 mm × 25 mm × 1 mm) was placed on the metal sheet of aluminium (Al) with a gap of dGA, which could be regulated by commercial tape (thickness of 0.05 mm, DELI Group Co., Ltd). An inexpensive and commercially available fibre laser system (SK-CX30, SK-Marker, China) was used for the LIBT technique to process the glass surface according to circular array pattern (diameter: 100 μm, spacing: 200 μm) with an area of 45 mm × 25 mm at ambient atmospheric pressure and room temperature. The process parameters included a frequency of 20 kHz, a scanning speed of 2000 mm/s, a laser fluence of 318.5 J/cm2, a pulse width of 100 ns, a focal diameter of 10 μm (focal length f: 19.45 cm) and an optical wavelength of 1064 ± 5 nm. Then the metal deposited glass surface was modified by 1 wt% fluoroalkylsilane (FAS, C8F13H4Si(OCH2CH3)3) ethanol solution to obtain a SHB surface. Fibre laser ablation was further conducted to form various complex SHL–SHB patterns on the glass substrate with the same process parameters as the LIBT technique.
Figure 1

Illustration of preparing the SHL–SHB pattern on glass substrate

Robustness and durability test

Falling sand abrasion and UV irradiation were conducted to test the robustness and durability of the prepared SHB surfaces, respectively. Sand grains (100 g, 0.3–0.9 mm in diameter) impinged on the tilted surfaces (45°) from a height of 25 cm with 7 cycles; prepared SHB samples were exposed to UV light (365 nm) for 24 h. Among the aforementioned tests, water contact angle (WCA) and sliding angle (SA) were measured. Tape peeling and fingerprint tests were carried out to investigate robustness of the SHB surfaces.


Water droplets of ~ 5 μL on samples were recorded by measurement (Krüss, DSA100, Germany) at ambient temperature, from which an average value was calculated from five different positions. The electron microscope (TV-60, China) was used to observe the variation of surfaces prepared by different gap distances dGA and output powers. The morphology and chemical element distribution were further observed by a scanning electron microscopy equipped with energy-dispersive X-ray (SEM and EDX, SUPRA 55 SAPPHIRE, Germany). Chemical composition was further characterized by an X-ray diffractometer (XRD, Empyrean, Holland, X-ray source (Cu Kα radiation (k = 0.15418 nm)) within the 5°–100° range at a scanning rate of 2θ = 0.026°/min and X-ray photoelectron spectroscopy (XPS, Thermo ESCALAB250Xi, American). Curve fitting of C 1s peak was operated by XPS peak 4.1 software with the C 1s peak at 284.6 eV as a reference.

Fog harvesting

To extend the application of SHL–SHB pattern on glass substrate, the pattern of wedge-shaped tracks (wedge angle of 7°) was prepared for harvesting the fog condensate. In a fog harvesting test (temperature: 20 ± 1 °C, RH: 80 ± 5%), the surfaces, including bare SHL, untreated glass, pristine Al surface, bare SHB and patterned glass, were vertically fixed at the holder. The culture dish was placed under the prepared sample for fog harvesting, as shown in Fig. 2. Fog was simulated by a household humidifier (Ultrasonic Nebulizer 402Al, moisture flow: ~ 3 mL/min), with a distance of 50 mm between the prepared surface and nozzle of the fog generator. Precision balance (resolution: 0.1 mg) was used to weigh the collected water for 20 min. A Sony camera (DSC-RX10M3, Japan) was used to record the aforementioned processes.
Figure 2

Illustration of fog harvesting

Results and discussion

Fabrication of extreme wetting patterns on an Al plate

The influences of gap distance dGA and output power on water contact angle (WCA) and sliding angle (SA) of the glass surface were firstly evaluated. As shown in Fig. 3 a1–a4 and b1–b4, the gap distance from 0.15 to 0.55 mm could all be used to obtain a SHB surface, where WCAs remained above 150° under the different output powers from 0.3 to 7.5 W, compared to untreated glass (19°) and pristine Al (70°). However, it was obvious that SAs would decrease with the descent of the gap dGA, among which the SA of SHB surface prepared by dGA of 0.15 mm and output power of 7.5 W reached 0° and water droplet could easily roll off from the 0-degree plane (Movie S1 and Figure S1 in the Supplementary Information). In addition, this surface also manifested more uniform morphology, as shown in Figure S2 of Supplementary Material, indicating that the surface was better treated compared with others. Furthermore, by fixing the output power of 7.5 W, samples prepared by dGA of 0 mm, 0.05 mm and 0.10 mm were then used to investigate the enhanced influence of dGA as shown in Fig. 3c. However, it was found that the glass receiver was bound to the donor Al substrate, which was inapplicable for further large-scale fabrication by LIBT technique due to instability in preparation. According to previous study [28], the processes of the LIBT technique can be attributed to donor material melting, vaporizing and ultimately depositing on the rear of the transparent glass receiver, facing the Al sheet. Thus, with the decrease in dGA, the intensive function of the LIBT processes would happen, resulting in the glass and Al sheet bonding together. Therefore, preparation parameters were fixed with dGA of 0.15 mm and output power of 7.5 W, unless specified otherwise.
Figure 3

WCAs (a1a4) and SAs (b1b4) of SHB surface on glass substrate fabricated by LIBT technique under the gap distance dGA of 0.15 mm, 0.25 mm, 0.35 mm, 0.55 mm with different output powers. c Influence of different gap distances (dGA) under the output power of 7.5 W

Due to the practical influence of sand-wind weather and the irradiation of sunlight, SHB glass substrate requires investigation for robustness and durability test by falling sand abrasion and UV irradiation. As illustrated in Fig. 4a-b and Movie S2 of Supplementary Material, the red-dyed droplet was observed to rapidly roll off from the tilted surface after the test. WCAs changed from 165° ± 3.1° to 155° ± 5.4° during 6 cycles test and finally dropped to approximate 147° after 7 cycles. In addition, SAs remained less than 10° during 6-cycle test while water droplet could not roll off after the 7th cycle, demonstrating robustness of SHB surface during 6-cycle falling sand test. It can be seen from the SEM images that little variation was found before and after the 6-cycle test, as shown in Fig. 4c. For the examination of UV resistance, the WCA still remained at 165° ± 3.3° after 24-h UV exposure, as shown in Fig. 4d and e. When the droplet contacted the UV-irritated SHB glass surface, easy detachment from SHB substrate could be observed, as shown in Fig. 4f. It was observed that the water droplets could still roll down from the surfaces after these tests including tape peeling and fingerprint tests, as shown in Movies S3 and S4 of Supplementary Information, demonstrating its good mechanical strength [29].
Figure 4

Robustness and durability test of the SHB surface. a, b Falling sand abrasion test and measured WCAs and SAs of 7 cycles. c The morphology of SHB surface before and after 6-cycle falling sand abrasion test. de UV resistance test and measured WCAs and SAs of 24 h. f Process of contacting and detachment on UV-irritated SHB glass surface

As a facile, green and rapid preparation method, inexpensive and commercially available fibre laser ablation was used to construct various complex SHL–SHB patterns such as Chinese characters, wedge-shaped tracks and folding fan pattern, as shown in Fig. 5a and b and Figure S3a of the Supplementary Material. SHL–SHB pattern was further characterized by SEM, as shown in Fig. 6a. Treated surface on glass substrate was characterized with hierarchical structures on the SHB area compared to the relative smooth morphologies of laser-treated area, demonstrating the function of laser ablation, as shown in Fig. 6 b1–b2 and c1–c2. The EDX elemental mapping of the patterned surface displayed the depletion of aluminium content (Fig. 6d), enrichment of oxygen content (Fig. 6e) and depletion of fluorine content (Fig. 6f), which confirmed a selective patterning by laser ablation for creating a SHL–SHB patterned glass substrate.
Figure 5

SHL–SHB pattern on glass substrate. a Chinese character. b Wedge-shaped tracks

Figure 6

Characterization of the SHL–SHB pattern on glass substrate. a SEM image. b1b2 SHB untreated area. c1c2 Laser-treated area. SEM–EDX mappings of the surface with elements d Al, e O, f F

Furthermore, from the XRD patterns of SHB region and SHL region, as shown in Fig. 7a, the diffraction peaks were assigned to Al2O3 and Al and referenced to JCPDS Card No. 052-0803 and No. 04-0787, respectively. The XRD pattern and cross-sectional view (Figure S3b of Supplementary Material) of the SHB region indicated that the glass surface was successfully deposited by donor materials during the process of the LIBT technique. After laser ablation treatment, most of the deposited layers were removed according to XRD pattern of SHL region. XPS spectra were also used to investigate the chemical composition of SHB untreated area and laser-ablated area as depicted in Fig. 7b, which were mainly composed of C 1s, O 1s, F 1s, Al 2p and Si 2p. The relative contents of O and F changed before and after laser treatment. For the SHB region, the relative contents of O and F were 34.3 and 24.6 at.%, respectively. At the SHL region, the O content increased to 49.0 at.%, while the F content plunged to 3.8 at.%, as shown in Figure S4 of Supplementary Material. Thus, the composition variation accounts for the patterned surfaces with wettability contrast. Figure 7c and d shows the high-resolution C 1 s peaks fitting results of the SHB region and the SHL region, which was deconvoluted into seven components including C–C bonds together with C–H and C–Si, which was centred at 284.6 ± 0.14 eV. The components at 286.1 ± 0.07 eV and 286.8 ± 0.03 eV were, respectively, attributed to C–O and CF2CH2 groups. The C = O group contribution was found at 288.6 ± 0.01 eV. A binding energy of 290.3 ± 0.07 eV was attributed to CF2–CH2 group. The peaks at 291.3 ± 0.01 eV and 293.7 ± 0.01 eV were assigned to –CF2 and terminal –CF3 moieties, respectively [30, 31]. As summarized in Table S1 of Supplementary Material, the SHB region contained about 37.6% –CF2 and 5.0% –CF3. In contrast, after laser ablation, the contents of –CF2 and –CF3 decreased to 0.2% and 2.6%, respectively, while C=O increased from 0.9 to 9.2%. Consequently, laser ablation treatment could rapidly obtain the observed SHL patterns on a SHB surface due to the reduction of hydrophobic F-containing groups and the increment of the hydrophilic O-containing groups.
Figure 7

Characterization of morphologies and chemical composition of the SHL–SHB pattern on glass substrate. a XRD patterns of SHB region and SHL region. b XPS spectra of elements. Peak-fitted high-resolution C 1s spectra of c SHB region and d SHL region

Inspired by the contrast wettability structures of the desert beetle [32], the prepared samples were firstly used for fog harvesting. As shown in Fig. 8a and b, it was obvious that condensing water droplet grew, merged into a larger droplet and finally formed a huge bump at the bottom of surface of the untreated glass and pristine (Movie S5 and S6 of Supplementary Material). In contrast, as shown in Fig. 8c, the bare SHL background manifested great fog adsorption capacity with water condensates spreading rapidly and forming film-like condensation areas in only 19 s. However, with a low rate of droplets proceeding, a huge bump was observed after water flowed downward (Movie S7 of Supplementary Material). For bare SHB background shown in Fig. 8d, dropwise condensation took place with condensing droplets growing, contacting with each other, merging into a large droplet and falling off from the surface (Movie S8 of Supplementary Material). By contrast, for wedge-shaped SHL–SHB pattern 1 (SSP1) with spacing distance of d1 (4 mm), nucleated droplet constantly grew and merged at SHB regions which were transported into SHL domains after contacting the border of SHL pattern. Driven by inner Laplace pressure gradient [33, 34, 35, 36], pumpless transportation of the condensing water took place at the SHL wedge-shaped track pattern (Movie S9 of Supplementary Material). As shown in Fig. 8e, neighbouring droplets at the tail end of tracks merged into a large droplet due to close spacing distance of 4 mm, demonstrating fast transition to film-like condensation. Wedge-shaped SHL–SHB pattern 2 (SSP2) with spacing distance of d2 (8 mm) is shown in Fig. 8f. However, condensing droplets rapidly shed off due to the gravity force with the droplet volume increasing and reaching the threshold value (Movie S10 of Supplementary Material), decreasing the water residual and realizing sustained droplet drainage.
Fig. 8

Fog harvesting. a Untreated glass. b Pristine Al substrate. c SHL background. d SHB background. e SHL–SHB pattern 1 with spacing distance of d1. f SHL–SHB pattern 2 with spacing distance of d2

Water condensates were then collected during fog harvesting for 20 min. For bare SHL background, only one droplet shed off, as shown in Fig. 9a. On the untreated glass substrate, pristine Al surface and bare SHB surface, condensing droplets took more time to converge and average departing droplet mass was 91.1 mg, 59.0 mg and 57.8 mg, respectively, which could hardly provide efficient droplet drainage. For the sample of SSP1 with spacing distance of 4 mm, 15 droplets with average mass of 158.0 mg were collected, which is too large to promote high efficiency of sustained drainage, compared to 70 droplets with average droplet mass of 50.4 mg for the sample of SSP2 (8 mm). Figure 9b shows bare SHL surface possessed the lowest efficiency of 1.78 mg cm−2 min−1, compared with untreated glass (3.64 mg cm−2 min−1) and pristine Al surface (8.71 mg cm−2 min−1). Due to the great pinning force on the wetted SHB surface, the fog harvesting efficiency was 10.26 mg cm−2 min−1. Influenced by the close spacing distance, SSP1 (4 mm) exhibited harvesting efficiency of 10.58 mg cm−2 min−1; while spacing distance increased to d2 (8 mm), condensing droplets could rapidly shed off and realized a new cycle of droplet drainage after growing beyond departing volume and exceeding the pining force of tail end, resulting in the highest fog harvesting efficiency of 15.68 mg cm−2 min−1. Compared with bare SHL background, untreated glass, pristine Al and SHB surface, this impressive fog harvesting ability of SHL–SHB wedge-shaped tracks pattern on glass substrate increases the harvesting efficiency by nearly 781%, 331%, 80% and 53%, respectively. A comparison between our work and the data found in previous studies is listed in Table S2 of Supplementary Information. It is evident that our work possesses a high water collection efficiency with this facile, cost-effective and non-corrosive preparation method. As shown in Fig. 9c, the influence of droplet volume on pumpless transportation was then investigated. When deposited on the front end of the wedge-shaped track with the distance of 23 mm, droplets of 35 μL would only take 238 ms to complete the transportation process (Movie S11 of Supplementary Material), while droplets of 5 μL needed 680 ms to complete the process. The results indicated that droplets of 5 μL and 35 μL could both rapidly reach the tail end of track driven by inner Laplace pressure gradient.
Fig. 9

Fog harvesting. a Harvesting droplet numbers and average droplet mass. b Fog harvesting efficiency. c Pumpless transportation process


We constructed SHL wedge-shaped patterns on robust and durable SHB glass substrates by using the LIBT technique, FAS modification and laser ablation, avoiding the use of mask technology and any hazard chemicals. This research could be an alternative way SHL–SHB patterns on glass substrates, which is not merely a promising candidate for water harvesting to alleviate he regional water shortage but also for microfluidic devices, droplet manipulation and cell screening.



This work was financially supported by the National Natural Science Foundation of China (NSFC, Grant No. 51305060) and National Basic Research Program of China (Grant No. 2015CB057304). F. Chen acknowledges the support from National Postdoctoral Program for Innovative Talents (No. BX20190233). I. P. Parkin acknowledges the support from EPSRC grant of Industrial Doctorate Centre: Molecular Modelling & Materials Science (EP/G036675/1). Yao Lu acknowledges the financial support from the QMUL-SBCS start-up.

Supplementary material

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Authors and Affiliations

  1. 1.Key Laboratory for Precision and Non-traditional Machining Technology of the Ministry of EducationDalian University of TechnologyDalianPeople’s Republic of China
  2. 2.Key Laboratory of Mechanism Theory and Equipment Design of Ministry of EducationTianjin UniversityTianjinPeople’s Republic of China
  3. 3.Department of Chemistry, School of Biological and Chemical SciencesQueen Mary University of LondonLondonUK
  4. 4.National Key Laboratory of Science and Technology on Helicopter TransmissionNanjing University of Aeronautics and AstronauticsNanjingPeople’s Republic of China
  5. 5.Department of ChemistryUniversity College LondonLondonUK

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