Materials & Design 185 (2020) 108236

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Materials & Design

journal homepage: www.elsevier.com/locate/matdes

Durable deicing lubricant-infused surface with photothermally

switchable hydrophobic/slippery property
Dequan Wu a, 1, Lingwei Ma a, 1, Fan Zhang a, Hongchang Qian a, Badar Minhas a,
Yumin Yang b, Xiao Han b, Dawei Zhang a, *
a
Beijing Advanced Innovation Center for Materials Genome Engineering, Institute for Advanced Materials and Technology, University of Science and
Technology Beijing, Beijing, 100083, China
b
School of Chemistry and Biological Engineering, University of Science and Technology Beijing, Beijing, 100083, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

The lubricant infused surface was

fabricated by infusing cocoa oil and
Fe3O4 into anodic aluminum oxide.

The lubricant could be melted by
heating at 46  C due to the photo-
thermal effect of Fe3O4.

The surface possessed low ice adhe-
sion (0.3 KPa) and efficient defrost/
deicing performance.

The melted lubricant repaired the
defects and the solid lubricant could
withstand fluid impact.

a r t i c l e i n f o a b s t r a c t

Article history: Lubricant infused surfaces (LISs) are promising platforms to address the icing problems, but their long-
Received 6 July 2019 term stability remains a significant challenge. In this study, a durable LIS with photothermal response
Received in revised form and reversible solid/liquid transformation was fabricated to rapidly thaw frost accumulation and reduce
23 September 2019
ice accretion. The newly designed LIS was manufactured by infusing low-melting cocoa oil and efficient
Accepted 24 September 2019
photothermal Fe3O4 nanoparticles into anodized aluminum oxide substrate. Upon irradiation with
Available online 15 October 2019
infrared light, the Fe3O4 nanoparticles could absorb light energy and melt the solid lubricant into slippery
liquid. The dual actions of surface heating and slipperiness of melted lubricant promoted the thawing of
Keywords:
Lubricant infused surface
frost/ice and de-adhesion of ice block. Additionally, the durability of LIS was strengthened by the
Photothermal combination of the self-healing effect of the melted lubricant, and the robustness of the solid state. The
Deicing hydrophobic lubricant diminished the lubricant loss during repeating freezing/unfreezing cycles and
Durability withstood longtime flowing water impact. The proposed concept of switchable hydrophobic/slippery
lubricant will advance the design of durable LISs and provide a promising LIS platform for deicing
application.
© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/).

1. Introduction

Ice accretion causes serious problems for industrial and resi-

dential facilities and structures, such as house roofs, power grid-
lines, heat exchangers, and transportation equipment, resulting in
* Corresponding author.
E-mail address: dzhang@ustb.edu.cn (D. Zhang). severe safety peril and economic losses [1]. Conventional strategies
1
These authors contributed to the work equally. to solve icing problems primarily involve chemical deicing, active

https://doi.org/10.1016/j.matdes.2019.108236
0264-1275/© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
2 D. Wu et al. / Materials & Design 185 (2020) 108236

heating, and mechanical tapping, which are often complicated, surface heating and slippery properties of melted lubricant pro-
costly and environmentally hazardous [2e6]. Among various vided the substrate with superior deicing performance. Addition-
deicing innovations, bionic coatings developed by mimicking ally, the melted lubricant was capable of healing defects, which
structures and chemical components of organisms have received further improved the mechanical durability of the LIS. In this paper,
intensive attention in recent years [7e11]. Inspired by Nepenthes the durability of the LIS was demonstrated through cycling tests,
pitcher plants, a concept referred as lubricant infused surface (LIS) including heating-cooling, icing-deicing, repeated abrasion, and
or slippery liquid infused porous surfaces (SLIPS), has been pro- exposure to flowing water for an extended period of time. This
posed to prevent ice accumulation by forming a lubricant layer work presents a design strategy for the development of durable
between the ice and substrate [12e15]. The lubricant layer delays slippery surfaces and provides a promising system for deicing
the ice nucleation time and minimizes the ice contact area on rough applications.
surfaces. Various liquids have been employed as the functional
lubricant, such as silicone oil, mineral oil, fluorinated Krytox oil, and 2. Materials and methods
ionic liquids [16,17]. These liquid-like lubricants coated on a nano-
textured substrate can form an ultra-smooth and chemically ho- 2.1. Materials
mogeneous interface [18,19], which are capable to minimizes the
ice contact area, eliminates the pinning spots on rough surfaces and High purity aluminum (99.999 wt%) was purchased from the
enables the easy removal of adhered ice block [20,21]. Contributing Beijing Institute of Nonferrous Metals (China). Iron(II) sulfate hep-
to their low surface energy and high movability, these liquid lu- tahydrate (FeSO4$7H2O, AR, >99.0%), iron(III) chloride hexahydrate
bricants also suppress ice formation by delaying the nucleation (FeCl3$6H2O, AR, >99.0%), and cocoa oil (C20H42, AR, >99.0%) were
time of water drops and then shedding them off before ice nucle- purchased from Aladdin Industrial Corporation. Sulfuric acid
ation, even for those condensation drops with small diameter (less (H2SO4, AR, >95.0%) and ethanol (CH3CH2OH, AR, >99.7%) were
than 600 mm) [22]. purchased from Sinopharm Group. Ammonia hydroxide solution
Although very promising anti-icing performance has been (NH3$H2O, AR, 25e28%) was provided by Shanghai Macklin
demonstrated using LIS/SLIPS, they suffer from limited durability Biochemical Co. Ltd. 1H,1H,2H,2H-Perfluorodecyltriethoxysilane
and poor longevity due to the inevitable loss of lubricant [23e25]. (PFDTES, C16H19F17O3Si, AR, >97.0%) was purchased from Sigma-
When exposed to external impacts such as abrasion [26,27], flow- Aldrich. Other chemical reagents were purchased from Sino-
ing water [28,29], and icing-deicing cycles [30], liquid lubricants pharm Group. Deionized (DI) water was used for all experiments.
are prone to drain away due to their high mobility and low surface
tension [31]. For example, a lubricant with low viscosity (12 cst) 2.2. Fabrication processes
may be lost more quickly than that with higher viscosity (140 cst)
under a shear force of flowing water [18]. The lubricant with Preparation of Fe3O4 nanoparticles (NPs). Fe3O4 NPs were
extremely low surface energy may cloak on the condensed liquid or prepared by a co-precipitation method, as showed in Scheme 1a1.
adhered ice cube and be removed by the sliding drops [23]. Even Briefly, 100 mL H2SO4 aqueous solution (0.5 mmol/L, pH ¼ 3),
under static conditions, such as long-term immersion or exposure, FeCl3$6H2O (5.41 g), and FeSO4$7H2O (2.80 g) were added to a
liquid lubricants dissolve or evaporate slowly and are lost little by three-necked flask. The solution was heated to 60  C and stirred for
little [32,33]. The lack of mechanical durability and chemical sta- 10 min to eliminate dissolved oxygen. Subsequently, ammonia hy-
bility results in the deterioration of the slippery property and droxide solution (25 vol%) was added dropwise (5 drops every
compromises the anti-icing function [34]. These seem to be an second) into the flask while stirring at 60  C under nitrogen until
irreconcilable contradiction: the high mobility and low surface the pH reached 11. After 1 h, Fe3O4 NPs were precipitated and
energy of the liquid lubricant enable the LIS with excellent water separated from the supernatant using an external magnet. Fe3O4
repellency and deicing behavior, whereas these properties also NPs were then placed in a new beaker and redispersed in DI water
cause the loss of lubricant under external impact. Therefore, repeatedly until the pH reached 7. The prepared Fe3O4 NPs were
imparting the LIS with both excellent durability and slipperiness or then thoroughly washed with ethanol.
deicing performance is a great challenge for practical applications Modification of Fe3O4 NPs with oleic acid. To improve the
of anti-icing LIS. stability and compatibility of Fe3O4 NPs in cocoa oil, the surface of
Previous studies have mainly focused on the optimization of the the Fe3O4 NPs was modified with oleic acid. The modification
durability of LISs on anti-icing surfaces through building delicate process is shown in Scheme 1a2. The prepared NPs (15 g) were
structures to retain the lubricant and improve the capillary dispersed in DI water (100 mL) in a three-necked flask with nitro-
attraction, or fabricating complex multilayers to supply the surface gen protection and stirred at 1000 r/min and 85  C. Ammonium
with continuous lubricant secretion [35,36]. However, few re- hydroxide (25 vol%, 5 mL) was then added to the flask dropwise
searchers have investigated how to improve the durability by until the pH reached 11, followed by addition of oleic acid (5 mL).
changing the flow properties of the lubricant itself, which is one of After stirring for 40 min, the precipitate was transferred to a new
the key factors to address the lubricant loss. beaker and washed with DI water for five times, and finally sepa-
In this work, we introduce for the first time, a lubricant with rated using an external magnet to obtain oleic acid modified NPs,
controllable solid/liquid phase transformation to prepare a LIS with named as Ol-Fe3O4.
desirable deicing performance and enhanced durability. The Preparation of photothermal responsive lubricant. As shown
lubricant was prepared by mixing low-melting cocoa oil with in Scheme 1a3, the prepared Ol-Fe3O4 (5 g) and cocoa oil (10 g) were
photothermal Fe3O4 nanoparticles (NPs) which possess high pho- mixed at 60  C and stirred at 300 r/min. The obtained product is
tothermal efficiency, controllable size and wide compatibility with referred to as photothermal responsive lubricant or NP-
lubricant. The lubricant was infused into anodic aluminum oxide lubricant.
(AAO) templates by vacuum impregnation [40]. The hydrophobic Fabrication of anodized aluminum oxide (AAO). AAO was
lubricant in solid state could withstand long-term environmental fabricated using a two-step anodization method. Firstly, electro-
impact and repeating ice-deice cycles at ambient temperature. polished aluminum foil was anodized at 210 V via a DC source
Upon irradiation with infrared (IR) light, owing to the photothermal (Keysight, N8741) in a 0.5 M phosphoric acid solution at 0  C with
effect of Fe3O4 NPs, the solid lubricant transformed into liquid that vigorous stirring. After removing the first oxide layer in an acidic
endowed the surface with slippery properties. The combination of solution (6.0 wt% phosphoric acid, 1.8 wt% chromic acid, and DI
 D. Wu et al. / Materials & Design 185 (2020) 108236 3

Scheme 1. (a) Preparation scheme of photothermal responsive lubricant: (a1) preparation of the Fe3O4 NPs by co-precipitation method; (a2) modification of the Fe3O4 NPs with
oleic acid; (a3) mixing the modified NPs with cocoa oil. (b) Schematic illustration of the fabrication process and application of the photothermal responsive lubricant infused
surface: (b1) fluoridation of the bare AAO by immersion of the specimens in a PFDTES solution; (b2) infusion of the prepared NP-lubricant into the modified AAO via a vacuum
immersion method; (b3) the deicing performance of melted NP-LIS. The surface heated by IR irradiation was melted into a slippery liquid surface, which efficiently reduces ice
adhesion. (b4) The lubricant in the solid state maintains high stability even when exposed to flowing water.

water) at 60  C for 30 min, a second anodization step was per- 2.3. Characterization
formed under the same condition for 20 min. The samples were
then treated using a pore broadening process in phosphoric acid Scanning electron microscopy (SEM, SU8020 Japan) was used to
solution (5.0 wt%) at 30  C for 20 min to obtain AAO with nanopore record top-view and cross-sectional images of the prepared spec-
diameter of 500e700 nm and depth of ~5 mm. imens. To investigate the smooth morphology of slippery LIS heated
Modification of AAO substrate with PFDTES. AAO substrates by IR irradiation, the melted specimens were solidified in liquid
were pretreated with PFDTES to improve the hydrophobicity and nitrogen before observation. Elemental mapping was evaluated by
compatibility [19,39]. As shown in Scheme 1b1, AAO substrates energy-dispersive X-ray spectroscopy (EDS; EMAX, HORIBA, Japan).
were immersed in the PFDTES solution (1 mL PFDTES, 8 mL The morphology of modified Fe3O4 NPs was characterized using a
deionized water, and 92 mL ethanol) for 30 min. Afterwards, the transmission electron microscopy (TEM; JEM-1200EX, Japan). X-ray
AAO samples were transferred to a dryer and heated at 150  C for diffractometry (XRD; D8 ADVANCE, Bruker) was used to investigate
1 h. These modified AAO substrates are referred to as PF-AAO. the crystal structure of the prepared Fe3O4 NPs. Fourier transform
Fabrication of photothermal responsive LIS. The photo- infrared spectroscopy (FT-IR; Nicolet iS10, Thermo Nicolet Corpo-
thermal responsive LIS was fabricated by infusing the NP-lubricant ration, America) was used to measure the components of the re-
into PF-AAO. The complete infusion of photothermal responsive action system in the vibrational frequency range from 4000 cm1 to
lubricant into PF-AAO (Scheme 1b2) was achieved through a vac- 400 cm1. Apparent Contact Angle (CA) was measured (Dataphysics
uum impregnation method as described in our previous study [40]. OCA20, Germany) by placing DI water droplets (~5 mL) onto the
Briefly, the PF-AAO samples were placed in a vacuum chamber prepared sample surfaces [41]. The CA of the melted surface was
(~3 Pa) for 5 h to completely remove air in the container and in the measured by first placing the water droplets on the surface and
nanopores. The chamber was then placed on a heater and the then heated with IR irradiation. The sliding angle (SA) was
temperature was set at 50  C. Melted NP-lubricant was then measured by placing a 10 mL water droplet on a specimen and then
injected into the container to coat the PF-AAO sample. After soak- tilting the surface slowly until the water droplet slides off. The re-
ing under vacuum for 1 h, the lubricant was infused in the nano- sults are the average values from five measurements on different
pores without resistance from compressed air trapped in the pores. areas of the samples.
After removing the substrate from the vacuum, the atmosphere can
further push the lubricant into the pores to achieve complete
impregnation. The fabricated photothermal responsive lubricant 2.4. Experimental methods
infused surface is referred as NP-LIS (nanoparticles and lubricant
infused surface). Heating method and temperature recording. A fiber coupled
Fabrication of normal LIS. To compare the durability between laser diode (ANJ Laser, China) was used to heat the film surface by IR
normal LIS and NP-LIS, the liquid mineral oil (Shell Advanced AX5, irradiation at 808 nm wavelength and working power ranging from
Shell Company) was used to impregnate into AAO by vacuum im- 0 W to 5 W. The diameter of the laser ranged from 1 to 5 mm by
mersion method to fabricate normal LIS, which has been reported adjusting the distance between the fiber and the surface. A ther-
previously [40]. modetector (HE802, HUATO Thermometry Co., China) was used to
record the temperature by attaching the sensor tightly to the film
4 D. Wu et al. / Materials & Design 185 (2020) 108236

surface. The sensor was carefully place to avoid being directly sparse distribution on the surface is the porous nanochannel. As for
irradiated by the IR laser. During heating and deicing testing, the IR the NP-lubricant, the surface is covered with cocoa oil and Fe3O4
laser with power of ~3 W was used to irradiate the surface of the NPs (Fig. 1d). The CA on the NP-LIS is ~135 , which is significantly
LIS. higher than that of bare AAO, reflecting the high hydrophobicity
Frosting and defrosting test. Specimens of 20 mm  20 mm and water repellency of NP-LIS [43,44]. As shown in the cross-
were placed on a homemade Peltier cooler, which was located in- sectional image of Fig. 1e, the nanochannels are completely
side a chamber. The relative humidity (RH) in the chamber was infused with photothermal responsive lubricant, indicating the
controlled to be 100% by venting moisture continuously. The high efficiency of vacuum impregnation. The fabricated NP-LIS film
specimens were cooled to 10  C at a cooling rate about 1  C/s. Fog is also confirmed by the distribution of Fe and C from EDS mapping
spray promoted frost generation; in order to remove the frost from (Fig. 1f). A clear boundary can be identified at the root segment of
the surface, IR light was introduced using a laser at a distance ~1 cm the nanochannel to distinguish the density and thin distribution
from the specimens. The frosting and defrosting processes were parts, which also confirms that the NP-lubricant is infused
recorded with a micro-lens camera. throughout the entire depth of the nanopores. Si is distributed
Ice adhesion strength measurement. A 10 mm  10 mm among the entire cross-section of NP-LIS, indicating the successful
cuvette filled with ~3 mL fresh DI water was inverted and placed on fluoridation of AAO with PFDTES.
the specimens. The temperature of the cooler was set at 10  C and
maintained for 24 h to ensure complete freezing of the water in the 3.2. Photothermal response
cuvette. The ice adhesion strength was measured in the cooling
chamber. The humidity in the chamber was decreased to ~10% to The transformation of the NP-LIS surface from the solid state to
avoid frost formation around the cuvette. The ice adhesion force the liquid state is caused by the surface temperature increase upon
was recorded by a dynamometer (NSCING, SH-200, China). The IR irradiation. The Fe3O4 NPs on the surface absorb light energy to
cuvette was pushed at a contact point less than 1 mm above the heat the surrounding cocoa oil. The melted cocoa oil then becomes
substrate. The measurements were repeated 5 times to obtain an transparent so that IR light can pass through the surface layer and
average value. activate the Fe3O4 NPs below it. In this manner, all the lubricant
Surface mechanical durability. The mechanical durability of efficiently melts into liquid.
the surface was evaluated using sandpaper (# 800) with abrasion To study the photothermal response, the specimen was placed
pressure of 2 kPa to scratch the surface. The abrasion distance was on a Peltier cooler with a controlled temperature of 10  C; the
2 cm in each cycle. After each abrasion test, the surface was healed surface temperature of NP-LIS was recorded by the sensor mounted
under IR laser irradiation. This abrasion-repairing cycle was on the film. Temperature increase as a function of time for the
repeated 10 times. untreated AAO and NP-LIS with different amounts of Fe3O4 NPs is
Flowing water washing test. Flowing water was used to wash shown in Fig. 2a. For bare AAO, the temperature did not increase
the specimens by placing the specimens in beaker with water since the IR irradiation is not available on AAO alone, whereas for
stirred at 1000 r/min above a magnetic agitator for 30 min. The NP-LIS, the surface temperatures increased rapidly from 10  C to
specimens were placed perpendicular to the direction of water flow ~0  C in 10 s, reaching a saturation temperature of 46  C in ~60 s.
to resist the power of fluid flush. NP-LIS surfaces with Fe3O4 contents of 10 wt%, 20 wt%, and 50 wt%
achieved maximum temperatures of 37  C, 42  C, and 45  C,
3. Results and discussion respectively, exceeding the melt temperature of cocoa oil (35  C).
After turning off the light, the surface temperature dropped
The fabrication process of the photothermal responsive LIS was remarkably to 10  C. To calculate the heating efficiency, IR irra-
introduced in detail in Section 2.2 and showed in Scheme 1. Briefly, diation at different powers was carried out on NP-LIS with speci-
the photothermal responsive lubricant is prepared and then mens containing different Fe3O4 contents. Fig. 2b shows that the
infused in porous AAO. Firstly, Fe3O4 NPs were prepared by a co- saturation temperature increases with irradiation power and Fe3O4
precipitation method. The Fe3O4 NPs were modified with oleic content. Alternate heating and cooling cycle tests were performed
acid to enhance the compatibility with cocoa oil. The microstruc- to evaluate the response time and attenuation of the surface tem-
ture and chemical composition of the treated Fe3O4 NPs were perature at subzero and room temperatures (Fig. 2c). The surface
analyzed by TEM, XRD, and FTIR (see Fig. S1). The photothermal temperature increased quickly from the initial temperature to its
responsive lubricant (NP-lubricant) was then prepared by mixing saturation temperature during the repeated heating-cooling cycles.
the NPs with melted cocoa oil. Secondly, to improve the surface No degradation of the heating ability was observed, indicating a
hydrophobicity of bare AAO and its compatibility with oil, the films recyclable photothermal response of the NP-LIS. Increasing the
were fluoridated by immersing in a fluoroalkylsilane solution temperature of NP-LIS from room temperature and the heating
(Scheme b1). Finally, the photothermal responsive lubricant efficiency under IR irradiation at different powers are also shown in
infused surface (NP-LIS) was fabricated by a vacuum impregnation Figs. S3a and S3b. The stable heating efficiency is attributed to the
method [40] to incorporate NP-lubricant into the AAO nano- coverage of cocoa oil on Fe3O4 particles, which avoids the oxidation
channels. The resulting NP-LIS meets the basic criterion of a stable of Fe3O4 during the heating process.
liquid infused surface (Fig. S2).
3.3. Surface wettability
3.1. Surface morphology
The wettability of the NP-LIS transformed from the solid state to
The morphology, wettability, and elemental distributions of the liquid state was investigated by SEM and measurement of the
bare AAO and NP-LIS are presented in Fig. 1. As shown in Fig. 1a and apparent contact angles as well as sliding angle. As shown in Fig. 3a,
b, bare AAO is composed of well-aligned empty nanochannels with after IR irradiation, the melted surface was much smoother than
diameters of ~700 nm and depth of ~5 mm. The CA on bare AAO is the solid surface (see Fig. 1a) and the CA was 122 . In Fig. 3b and
~80 , reflecting its poor water repellency [42]. As the EDS mapping Movie S1, the water droplet pinning on the surface began to slide
of the bare AAO shows (Fig. 1c), only Al is detected, and there is a off after 8s of IR irradiation. Fig. 3d further introduced the SA of
clear boundary between the two distinct structures: the dense water droplets with different volumes on solid and melted surface.
distribution at the bottom is the aluminum substrate, and the The sliding angles decreased as the volumes of water drops grew
 D. Wu et al. / Materials & Design 185 (2020) 108236 5

Fig. 1. SEM images and EDS mapping of (aec) the untreated AAO and (def) prepared NP-LIS. (a) Top view of the AAO substrate (pore diameter 500e700 nm). The inset image is the
CA of the bare AAO; (b) cross-section of AAO (ordered arranged nanochannel depth ~ 5 mm); (c) EDS mapping of the distribution of Al, Fe, Si, and C. Only Al was detected; (d) top
view of NP-LIS. The inset image is CA of NP-LIS; (e) cross-section of NP-LIS (the nanochannel is fully infused with NP-lubricant); (f) EDS mapping of the distribution of Al, Fe, Si, and C
of NP-LIS, also indicating the full impregnation of the porous substrate.

Fig. 2. Photothermal response characteristics of the NP-LIS. (a) Increasing temperature process recorded for the bare AAO and NP-LIS with different Fe3O4 NPs content (10%, 20%,
30%, and 50%) with light on, and then when the light is switched off. (b) Saturation temperatures of the NP-LIS heated by IR irradiation at different powers. (c) Repeated heating/
cooling cycles applied to the NP-LIS.

up. In Fig. 3c and Movie S2, a variety of liquid droplets (i.e., milk, demonstrating the slippery property and enhanced dewetting
ink, blood, and ethanol) condensed on the surface shed off after IR performance of the melted surface. The SA remained constant for
irradiation. The CA and SA of NP-LIS during several heat-cooling both solid and liquid states during the repeated melting/freezing
cycles are shown in Fig. 3e. The SA decreased dramatically from cycles, indicating the desirable stability of the NP-LIS.
~63 to ~4.8 when the surface transformed from solid to liquid, Supplementary data related to this article can be found at
6 D. Wu et al. / Materials & Design 185 (2020) 108236

Fig. 3. Wetting behavior of NP-LIS transformed from the solid state into the liquid state. (a) SEM image and CA (inset) of NP-LIS in the melted state (frozen in liquid nitrogen to
observe the surface). (b) A water droplet was pinning on the NP-LIS surface initially and sliding off after IR irradiation. (c) Liquid droplets (milk, ink, blood, and ethanol) shed off from
the slippery surface. (d) Sliding angle of testing water droplets with different volumes on solid and melted NP-LIS. (e) CA and SA measured for NP-LIS during melting/freezing cycles.

https://doi.org/10.1016/j.matdes.2019.108236. and completely melted into water droplets after irradiation for 30 s.
The small water drops would condense into large droplets and shed
3.4. Defrosting performance off quickly from solid surface. Because of the stability of the solid
phase, the lubricant was hardly impacted by the sliding drops.
The defrosting properties of normal LIS, deteriorated LIS, bare These results demonstrated that normal LIS was not capable of
AAO and NP-LIS were investigated by defrost test using a Peltier preventing frost nucleation for a long time, whereas the NP-LIS
cooler at 10  C in a hygrothermostat chamber with continuous fog could achieve a durable defrost property due to the efficient sur-
spray. Fig. 4a shows the frost results of normal LISs in different face heating and slipperiness of melted lubricant that shed off the
deterioration stages. The specimens were frozen for 10 min to thawed frost, as well as the robust of infused solid lubricant to
ensure the nucleation time. From number 1 to 5, the degradation diminish the oil loss.
increased by flowing water washing (water stirred at 1000 r/min, as Supplementary data related to this article can be found at
described in Section 2.4) for 10 min after each stage to accelerate https://doi.org/10.1016/j.matdes.2019.108236.
the loss of lubricant. For the as-prepared LIS (Fig. 4a1), only sub-
cooled water condensations were observed because the freezing 3.5. Deicing performance
point of water drops was decreased and their nucleation time was
prolonged by the infused liquid lubricant [20,21]. The movement of The deicing performances of ice block on normal LIS, deterio-
water drops carried away the volume [25]. As more and more water rated LIS, bare AAO, solid NP-LIS and melted NP-LIS were investi-
drops shed off through these surfaces in the repeating freeze- gated. The specimens with water droplets on the surface were
unfreeze cycles, the liquid lubricant lost and the rough substrate placed on a Peltier cooler at 10  C in a chamber with atmosphere
exposed, leading to the sticky of water drops and subsequent ice temperature of 0  C for 24 h to ensure the complete frozen of water
nucleation, as the scheme showed in Fig. 4d1 and 4d2. In Fig. 4a3, droplets. Ice adhesion strength was determined by measuring the
the frosts started to grow on the surrounding corner. For further ice detachment force via pushing over the ice columns frozen on
deterioration (Fig. 4a4 and 4a5), the tiny water condensations the surface, as described in Section 2.4. In Fig. 5a, the fresh LIS
transformed into a thin ice film. Owing to the loss of lubricant, the exhibited excellent deicing property that ice block could fall down
LIS failed to prevent the ice accumulation finally. The frost accu- by shaking the specimens as the ice adhesion strength was
mulation processes on bare AAO are showed in Fig. 4b and Movie measured to be 0.2 KPa in Fig. 5f. After flowing water washing for
S3. Due to the anchoring effect of moisture, frost accumulation 60 min, the LIS was deteriorated because the lubricant covered on
dramatically occurred on the bare AAO after freezing for 200 s surface lost. As shown in Fig. 5b, the ice blocks pinning on the
[45,46]. Upon IR irradiation, however, the frost remained on the deteriorated LIS could not be removed easily as the adhesion
surface because the empty AAO does not respond to the irradiation strength increased remarkably to 37.8 KPa in Fig. 5f. These agreed
and the temperature remained below 0  C. Fig. 4c and Movie S4 with the results we discussed above that the rough surface exposed
display the frost accumulation and defrost processes on NP-LIS. and ice nucleation wedged into the texted structure. For bare AAO,
Frost was also generated on the surface after freezing for 200 s, the ice adhesion strength was as high as 57.8 KPa due to the rough
 D. Wu et al. / Materials & Design 185 (2020) 108236 7

Fig. 4. The accumulation of frost on LIS, deteriorated LIS, bare AAO, and NP-LIS, as well as the defrost process of bare AAO and NP-LIS. (a) Frost/ice accumulation on LIS with different
deteriorated stage. (b) Frost on the bare AAO was hardly removed under IR irradiation. (c) Frost on the NP-LIS film was thawed in 30 s upon IR irradiation (power 3 W). (d) schematic
of frost nucleation on deteriorated LIS and deicing process of NP-LIS.

substrate. The deicing process of the bare AAO is illuminated in environment. In this way, most of the lubricant was remained in
Fig. 5c and Movies S5. Upon IR irradiation for 40 s, the water solid state in the porous substrate. Due to the excellent dewetting
droplets still frozen on the surface and no change occurred on the property and low ice adhesion strength of the solid lubricant sur-
bare AAO. In Fig. 5f, the NP-LIS displayed a very low ice adhesion face, the melted frost/ice would slide off from the NP-LIS without
force of 7.3 kPa. The distinct reduction of ice adhesion was related to deterioration problem. Therefore, the excellent deicing perfor-
the smooth topography and plasticity of the infused lubricant. The mance of NP-LIS was attributed to the dual functions of efficient
lubricant filled up the porous nanostructure and formed a smooth photothermal effect and dewetting property of NP-LIS, and the
surface, preventing the penetration of water and reducing the an- enhanced durability was attributed to the robustness of lubricant in
chor of ice into nanotextures. Owing to the hydrophobicity and solid state.
plasticity of the solid lubricant, slippage occurred easily at the Supplementary data related to this article can be found at
interface between ice and the LIS. As shown in Fig. 5d, ice chunks https://doi.org/10.1016/j.matdes.2019.108236.
could be fell off from the NP-LIS just by bending the specimen Repeated icing/deicing cycling reflects the durability of the
slightly. After IR irradiation (3 W for 30 s) in Fig. 5e and Movie S6, deicing performance. For the normal LIS, the longtime deicing
the root of the ice blocks and the contact area of the lubricant were processes often cause the loss of lubricant and the collapse of
thawed immediately and the adhesion strength reduced remark- surface structure [47]. As shown in Fig. 5g, the ice adhesion strength
ably from 7.3 kPa to 0.3 kPa (Fig. 5f). The melting spot of frost/ice on normal LIS increased from 0.2 KPa to 37.8 KPa gradually. For the
and underneath lubricant was only limited within the IR irradiation melted NP-LIS, the ice adhesion strength remained constant and no
area. The melting occurred not in the whole surfaces of specimen, degradation was observed during longtime icing/deicing cycling
but only the area of IR light spot. After irradiation, the melted testing. This improved durability was attributed to the efficient
lubricant solidified immediately at the low temperature photothermal deicing performance and stability of lubricant in
8 D. Wu et al. / Materials & Design 185 (2020) 108236

Fig. 5. Ice accumulation and deicing process of LIS, deteriorated LIS, bare AAO, solid NP-LIS and melted NP-LIS. (a) Frozen ice drops shed off from the fresh LIS by gravity. (b) Ice
pinning on the deteriorated LIS. (c) Ice blocks are not thawed after IR irradiation. (d) Ice blocks can be removed easily from NP-LIS by bending the specimen. (e) Icing removed from
the NP-LIS after IR irradiation for 40s. (f) Ice adhesion strength for LIS, deteriorated LIS, bare AAO and NP-LIS before and after IR irradiation. (g) Ice adhesion strength measured on
LIS and NP-LIS during repeated melting-freezing cycles.

solid state that diminished the loss of lubricant. The mechanical durability of the NP-LIS against force impact was
also assessed by repeated sandpaper abrasion tests at a load pressure
of 2 kPa and a friction track of 2 cm each time. The SEM images in
3.6. Durability
Fig. 7a and b shows the repair effect of the NP-LIS surface treated by
IR irradiation after abrasion. As shown in Fig. 7a, the scratched NP-
The mechanical durability of the LIS against physical damage is
LIS became rough, but after IR irradiation, the cracked NP-LIS sur-
significant for practical applications [27,48]. The AAO surface with a
face was repaired and largely recovered to become flat again
brittle nanoporous structure is vulnerable to cracking or other de-
(Fig. 7b), which resulted from the flowing of melted lubricant to the
fects caused by wear, repeated icing/deicing cycles, and other force
defects and reformation of the smooth surface. To evaluate the stable
impacts. According to a previous report, the LIS possessed a self-
wettability of the robust photothermal responsive LIS, the CA and SA
healing ability originating from the mobility of the liquid-like
of NP-LIS in different stages involving abrasion, melting to slippery
lubricant which could flow into cracks and cure the damaged sur-
surface, and solidification were recorded during the repeated cycles,
face spontaneously [38]. In this work, the nanochannels were filled
as shown in Fig. 7c. The CA of the worn surface increased from ~75
with solid lubricant that also had the possibility of melting into a
to ~126 after IR irradiation and stayed at ~120 upon cooling to
liquid and healing the defects. To investigate the self-healing effect
resolidification. The SA of the worn surface was greater than 90
of the NP-LIS specimen, artificial surface cracks were prepared by
(water droplets on the surface). After IR irradiation, the surface was
bending the specimen around a 5 mm diameter cylinder rod, fol-
repaired and the SA dropped to 6 . During the entire melting/so-
lowed by direct SEM observation of the defects before and after IR
lidification cycle, the CA and SA of the worn surface displayed rapid
irradiation. As shown in Fig. 6a and b, the NP-LIS surface was
and recyclable changes. No degradation of the surface wettability
broken into pieces with cracks of widths ranging from a few mi-
was observed, indicating the durability of the NP-LIS due to
crometers to dozens of micrometers, and the CA decreased from
remelting of the photothermal responsive lubricant.
135 to 102 . After IR irradiation, most of the cracks were healed,
The durability of NP-LIS compared with the lubricant-coated flat
the rough surface became smooth (Fig. 6c), and the CA increased to
aluminum was investigated in Fig. S4. Repeated sandpaper abrasion
130 , indicating the return of surface hydrophobicity. Magnification
tests demonstrated that the solid lubricant was easily removed
of the repaired cracks in Fig. 6d shows that the crack was refilled
from the flat aluminum foil as the weak adhesion of lubricant on
with lubricant and that the exposed aluminum substrate was
the smooth substrate. The NP-LIS was intact and undamaged after
recovered. As illustrated in Fig. 6e, the self-healing mechanism of
testing for ten times (Fig. S4b) due to the considerable hardness of
the solid lubricant was achieved by melting to reshape the rough
the porous oxide [49,50].
topography by flowing into the defects.
 D. Wu et al. / Materials & Design 185 (2020) 108236 9

Fig. 6. SEM images of NP-LIS with artificial cracks and self-healed surface. (a) Cracks and exposed substrate on the NP-LIS; (b) Magnification of the crack in (a); (c) cracks were
healed and the surface recovered to become smooth again after IR irradiation; (d) magnification of the repaired crack, demonstrating the flow of lubricant into the defects; (e)
scheme to illustrate the self-healing mechanism of the photothermal responsive lubricant surface.

To further probe the stability of the NP-LIS in the solid state, the and SA of ~5 ). Repeated irradiation/cooling cycles showed that the
NP-LIS and normal LIS were tested by immersion in stirring water surface temperature, morphology, and wettability of NP-LIS were
(1000 r/min) for 30 min. As shown in Fig. 7d, for normal LIS, the CA reversible. The enhanced defrosting performance and low ice
decreased and SA increased remarkably under flowing water for adhesion strength (0.3 kPa) were attributed to the combination of
about 10 min, indicating the loss of lubricant under shear force of the generated heat and slippery property of melted lubricant.
fluid [28]. For NP-LIS, the CA and SA maintained at ~132 and ~6 , Additionally, the film possessed high mechanical durability due to
respectively, indicating the stability of solid surface. Therefore, we the self-healing effect of the lubricant in the liquid state and the
demonstrate that the prepared NP-LIS possesses excellent me- high stability of the lubricant in the solid state. The damaged sur-
chanical durability due to the phase switchable lubricant, which face and deteriorated wettability could be recovered after repeated
protects the surface from physical impact in the solid state and can abrasion test due to the melted lubricant that flowed into the
act to self-heal any generated damage in the melted liquid state. To cracked and reformed a smooth surface. The solid lubricant could
further compare the durability of melted lubricant coated on flat withstand the sliding of thawed frost/ice and long-term impact of
aluminum and infused in AAO surface under water flowing con- flowing water, remaining the CA and SA steady. This switchable
dition, the two specimens were heated and employed with surface may provide new insights into the design and development
repeated water dripping (volume of 40 mL/min), as shown in of the next generation of anti-icing coatings.
Fig. S4c, after dripping for 20 min, the lubricant layer on aluminum
foil drained away partially due to the removal of shedding droplets.
Data availability
While for LIS, the lubricant was still stored intact in the nanopores
due to the capillary force of porous substrate (Fig. S4d).
The raw/processed data required to reproduce these findings
will be shared upon request.
4. Conclusions
CRediT authorship contribution statement
A solid-liquid switchable LIS with efficient deicing performance
and mechanical durability was developed by infusing low-melting Dequan Wu: Conceptualization, Investigation, Methodology,
cocoa oil and Fe3O4 nanoparticles into porous AAO substrate. Writing - original draft. Lingwei Ma: Investigation, Methodology,
Attributing to the high photothermal effect of Fe3O4 nanoparticles Writing - original draft, Writing - review & editing. Fan Zhang:
which absorb the energy of IR irradiation, the solid lubricant under Investigation. Hongchang Qian: Investigation. Badar Minhas:
environment temperature of 10  C was heated to a saturation Investigation. Yumin Yang: Investigation. Xiao Han: Investigation.
surface temperature of ~45  C, melting into a smooth liquid surface Dawei Zhang: Conceptualization, Methodology, Writing - original
with high hydrophobicity and slippery performance (CA of 122 draft, Writing - review & editing.
10 D. Wu et al. / Materials & Design 185 (2020) 108236

Fig. 7. Mechanical stability of the NP-LIS upon abrasion and exposure to flowing water. (a) SEM image of NP-LIS after sandpaper abrasion for 10 times under a load pressure of 2 kPa
and friction track of 2 cm. (b) The worn surface was healed and recovered with a smooth lubricant film after applying IR irradiation. (c) The CA and SA of NP-LIS measured after
abrasion, remelting, and solidification during repeated abrasion/repair cycles. (d) The CA and SA of normal LIS as well as NP-LIS measured during exposure to flowing water (1000 r/
min).

Acknowledgement [9] S. Zheng, C. Li, Q. Fu, W. Hu, T. Xiang, Q. Wang, M. Du, X. Liu, Z. Chen,
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This work is supported by National Natural Science Foundation (2016) 261e270.
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