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All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

A Critical Review of the Measurement of Ice Adhesion to Solid Substrates

Ice adhesion is an issue spanning a wide range of technical fields. In the aerospace industry, ice accretion has led to a large number of casualties and costs the industry billions of dollars every year. To design effective anti-/de-icing systems, the adhesion of ice to surfaces must be understood. In this review paper, the authors surveyed for papers providing methods for the measurement of ice adhesion. 113 papers were identified for comparison, with data being extracted from 58 papers with common test surfaces (aluminum, steel, Teflon® (Chemours), and polyurethane). The methods used were categorized and data were compared based on their precision and the trends they demonstrated. Conceptual problems were identified with the tests used in the literature and discussed, and open questions relevant to testing the adhesion of ice were identified. Several key parameters affecting ice adhesion identified from the literature were temperature, surface roughness, strain rate, and impact velocity. Their effects on adhesion strength were discussed. While researching this topic, it was discovered that many papers did not report the strain rate in their tests, and the vast majority of papers did not correct their data for stress concentrations on the surface, either of which has been shown to cause variation in the data by one order of magnitude. Data compared from the literature typically spanned one to three orders of magnitude. The causes of these variations were discussed.

Andrew H. Work↗
NASA NTRS2008

Coating Reduces Ice Adhesion

The Shuttle Ice Liberation Coating (SILC) has been developed to reduce the adhesion of ice to surfaces on the space shuttle. SILC, when coated on a surface (foam, metal, epoxy primer, polymer surfaces), will reduce the adhesion of ice by as much as 90 percent as compared to the corresponding uncoated surface. This innovation is a durable coating that can withstand several cycles of ice growth and removal without loss of anti-adhesion properties. SILC is made of a binder composed of varying weight percents of siloxane(s), ethyl alcohol, ethyl sulfate, isopropyl alcohol, and of fine-particle polytetrafluoroethylene (PTFE). The combination of these components produces a coating with significantly improved weathering characteristics over the siloxane system alone. In some cases, the coating will delay ice formation and can reduce the amount of ice formed. SILC is not an ice prevention coating, but the very high water contact angle (greater than 140 ) causes water to readily run off the surface. This coating was designed for use at temperatures near -170 F (-112 C). Ice adhesion tests performed at temperatures from -170 to 20 F (-112 to -7 C) show that SILC is a very effective ice release coating. SILC can be left as applied (opaque) or buffed off until the surface appears clear. Energy dispersive spectroscopy (EDS) and x-ray photoelectron spectroscopy (XPS) data show that the coating is still present after buffing to transparency. This means SILC can be used to prevent ice adhesion even when coating windows or other objects, or items that require transmission of optical light. Car windshields are kept cleaner and SILC effectively mitigates rain and snow under driving conditions.

Smith, Trent↗
NASA NTRSDate not supplied

Impact Ice Adhesion at NASA Glenn: Current Experimental Methods and Supporting Measurements

When examining the literature on the adhesion strength of impact ice, there have been a wide range of methodologies tried to measure the required stresses to induce interfacial delamination. Utilizing the Icing Research Tunnel at the NASA Glenn Research Center to generate the impact ice required for this work, several different mechanical tests have been and are being developed to determine the stresses along the interface between ice and coupon. This set of tests includes the technical mature modified lap joint test which has been used to conduct ice adhesion studies through a wide sweep of icing conditions. To conduct in situ ice adhesion measurements inside of the Icing Research Tunnel, several new experiments are currently being developed to make ice adhesion measurements during and immediately after ice accretion. In addition to these experimental methods, several supporting measurement techniques have been developed to allow for a better understanding on the influence of icing cloud conditions on the mechanical behavior of impact ice. Digital image correlation has been successfully implemented to augment the data generated by the modified lap joint test with full field surface displacement and strain measurements which allow for insight into the deformation processes present during a test. Both optical microscopy of impact ice samples along with ice replication techniques have been used to study the grain structure of the impact ice. This has led to a deeper understanding of the results from the modified lap joint method and how the structure of impact ice changes as it is accreted during an icing spray. The freezing process of impact ice generated by supercooled liquid water is not a volume conserving process, which leads to the presence of residual strains along the interface between ice and substrate. These strains have been observed using both a simplified flat geometry and a representative airfoil. The data gathered by these experimental adhesion methods and supporting measurements allows for a comprehensive understanding on the behavior of impact ice which will be critical to the development of future ice shedding models.

Ice Adhesion↗
NASA NTRSDate not supplied

Impact Ice Adhesion at NASA Glenn: Current Experimental Methods and Supporting Measurements

When examining the literature on the adhesion strength of impact ice, there have been a wide range of methodologies tried to measure the required stresses to induce interfacial delamination. Utilizing the Icing Research Tunnel at the NASA Glenn Research Center to generate the impact ice required for this work, several different mechanical tests have been and are being developed to determine the stresses along the interface between ice and coupon. This set of tests includes the technical mature modified lap joint test which has been used to conduct ice adhesion studies through a wide sweep of icing conditions. To conduct in situ ice adhesion measurements inside of the Icing Research Tunnel, several new experiments are currently being developed to make ice adhesion measurements during and immediately after ice accretion. In addition to these experimental methods, several supporting measurement techniques have been developed to allow for a better understanding on the influence of icing cloud conditions on the mechanical behavior of impact ice. Digital image correlation has been successfully implemented to augment the data generated by the modified lap joint test with full field surface displacement and strain measurements which allow for insight into the deformation processes present during a test. Both optical microscopy of impact ice samples along with ice replication techniques have been used to study the grain structure of the impact ice. This has led to a deeper understanding of the results from the modified lap join method and how the structure of impact ice changes as it is accreted during an icing spray. The freezing process of impact ice generated by supercooled liquid water is not a volume conserving process, which leads to the presence of residual strains along the interface between ice and substrate. These strains have been observed using both a simplified flat geometry and a representative airfoil. The data gathered by these experimental adhesion methods and supporting measurements allows for a compressive understanding on the behavior of impact ice which will be critical to the development of future ice shedding models.

Ice Adhesion↗
NASA NTRS2016

Effect of Molecular Flexibility upon Ice Adhesion Shear Strength

Ice formation on aircraft surfaces effects aircraft performance by increasing weight and drag leading to loss of lift. Current active alleviation strategies involve pneumatic boots, heated surfaces, and usage of glycol based de-icing fluids. Mitigation or reduction of in-flight icing by means of a passive approach may enable retention of aircraft capabilities, i.e., no reduction in lift, while reducing the aircraft weight and mechanical complexity. Under a NASA Aeronautics Research Institute Seedling activity, the effect of end group functionality and chain length upon ice adhesion shear strength (IASS) was evaluated with the results indicating that chemical functionality and chain length (i.e. molecular flexibility) affected IASS. Based on experimental and modeling results, diamine monomers incorporating molecular flexibility as either a side chain or in between diamine functionalities were prepared, incorporated into epoxy resins that were subsequently used to fabricate coatings on aluminum substrates, and tested in a simulated icing environment. The IASS was found to be lower when molecular flexibility was incorporated in the polymer chain as opposed to a side chain.

Smith, Joseph G.↗
NASA NTRS2019

The Effect of Stainless Steel 304 Surface Roughness on Ice Adhesion Shear Strength of Accreted Impact Ice

Aircraft in-flight icing is problematic due to the ad-verse effect on vehicle performance. It occurs when supercooled water droplets (SCWD) present in clouds, under the appropriate environmental conditions, col-lide with the aircraft surface resulting in accretion of ice (i.e., impact icing). Impact ice can range from clear/glaze to rime or a combination of the two (i.e., mixed) with the type determined by the air temperature (0 to -20°C), liquid water content (LWC, 0.3-0.6 g/cu.m), and droplet size [median volumetric diameter (MVD) of 15-40 µm] present during accretion.1 These impact icing events generally occur at temperatures ranging from 0 to -20°C. Below -20°C, ice crystals dominate the environment and typically do not adhere to the aircraft surface. A main difference between an impact icing occurrence and a slow growth icing (i.e., freezer ice) one is the speed of the icing event. Besides environmental conditions, ice adhesion strength (IAS) to a metallic substrate depends upon surface roughness. It is known that increasing surface roughness and decreasing temperature lead to in-creases in IAS.

Smith, Joseph G., Jr.↗
NASA NTRSDate not supplied

In-Situ Ice Adhesion Testing using the Deformed Skin Adhesion Test

There exists a plethora of ice adhesion testing methods such as centrifuge-based methods, push/pull methods, and lap joint shear tests. However, these methods often cannot be done in-situ during an icing spray and require researcher handling/preparation prior to testing. Additionally, many of these methods test ice accretions that are not representative of the ice shapes that grow on airframes which can have unintended consequences such as edge or corner stress concentrations. In order to mitigate the issues present with other ice adhesion tests a novel, hands-free, in-situ test method imbedded into the leading edge of the airfoil has been developed and tested in the NASA Glenn Research Center Icing Research Tunnel. The mechanics of the new test method are discussed with finite element simulations being used to highlight the fundamental mechanics of this test method. The testing procedures used during the experimental test campaign are discussed along with the icing cloud test matrix. Analysis of the force-displacement results highlights the repeatability of the test method with regards to both sample behavior across several days of testing and different ice shapes. The results from first run of the day showed a significant discrepancy from subsequent runs and differential image analysis was used to determine differences in the interfacial bonding states between runs.

Ice Adhesion↗
NASA NTRSDate not supplied

In-Situ Ice Adhesion Testing using the Deformed Skin Adhesion Test

There exists a plethora of ice adhesion testing methods such as centrifuge-based methods, push/pull methods, and lap joint shear tests. However, these methods often cannot be done in-situ during an icing spray and require researcher handling/preparation prior to testing. Additionally, many of these methods test ice accretions that are not representative of the ice shapes that grow on airframes which can have unintended consequences such as edge or corner stress concentrations. In order to mitigate the issues present with other ice adhesion tests a novel, hands-free, in-situ test method imbedded into the leading edge of the airfoil has been developed and tested in the NASA Glenn Research Center Icing Research Tunnel. The mechanics of the new test method are discussed with finite element simulations being used to highlight the fundamental mechanics of this test method. The testing procedures used during the experimental test campaign are discussed along with the icing cloud test matrix. Analysis of the force-displacement results highlights the repeatability of the test method with regards to both sample behavior across several days of testing and different ice shapes. The results from first run of the day showed a significant discrepancy from subsequent runs and differential image analysis was used to determine differences in the interfacial bonding states between runs.

Ice Adhesion↗
NASA NTRS2018

Design and Development of a Laboratory-Scale Ice Adhesion Testing Device

When an aircraft traverses through clouds containing supercooled water droplets, in-flight icing can occur that negatively affects vehicle performance by increasing weight and drag leading to loss of lift. Super-cooled water droplets present in clouds that impact vehicle surfaces can lead to inflight icing any time during the year.1 Most events occur at temperatures ranging from 0 to -20degC. Ice generated on the aircraft can vary between clear/glaze, rime, and mixed (Fig. 1) depending on air temperature (-5 to -20degC), liquid water content (0.3-0.6 g/m3), and droplet size (median volumetric diameter of 15-40 μm). Current strategies to remove ice are based on active technologies such as pneumatic boots, heated surfaces, and deicing agents (i.e., ethylene- and propylene-based glycols). The latter have potential environmental concerns. A passive approach to mitigate accreting ice that is actively being investigated are protective coatings. An ice mitigating coating could potentially be used as a stand-alone material, but more likely in combination with an active approach. In the latter scenario, potential reduction in power consumption by the active approach may be realized. To determine the ice adhesion strength of impact ice that is representative of the aircraft environment is not a trivial matter. Test methods utilizing slowly formed ice (i.e., freezer ice) do not accurately simulate this environment. Likewise, some testing methodologies involve sample relocation from the icing environment to the test chamber that can result in thermal shock to the sample, thus affecting the results. The Adverse Environment Rotor Test Stand (AERTS) located at Pennsylvania State University (PSU) has been demonstrated to simulate impact icing conditions within the icing envelope for the determination of ice adhesion shear strength (IASS) without removal/relocation of the sample.2 Due to the confidence in results obtained from AERTS, this instrument is in high demand and requires a significant amount of lead time and capital investment to obtain IASS results. As a solution for quickly and economically screening coatings in a controlled manner under impact icing conditions, a laboratory-scale ice adhesion test and dead blades were then removed from the rotor/blade assembly to obtain the final mass. The IASS of the live blade was determined from the difference in mass (before and after testing) of the live and dead blades, the ice shed area, and the rpm of the shed event. The same live blade sample was tested in triplicate at all three test temperatures. Surface roughness was determined using a Bruker Dektak XT Stylus Profilometer. Measurements were conducted using a 12.5 μm tip at a vertical range of 65.5 μm with an applied force of 3 mg. Data were collected over a 1.0 mm length at a resolution of 0.056 μm/point. Five single line scans at different locations were collected and processed using a two-point leveling subtraction. The resultant Ra (arithmetic roughness) and Rq (root mean square roughness) average values were calculated.

Smith, Joseph G., Jr.↗
NASA NTRS2020

Effects of Hydrogen Bonding and Molecular Chain Flexibility of Substituted n-Alkyldimethylsilanes On Impact Ice Adhesion Shear Strength

The effects of hydrogen bonding and molecular flexibility upon ice adhesion shear strength were investigated using aluminum substrates coated with substituted n-alkyldimethylalkoxysilanes. The location of the chemical group substitution was on the opposing end of the linear n-alkyl chain with respect to silicon. Three hydrogen-bonding characteristics were evaluated: 1) non-hydrogen bonding, 2) donor/acceptor, and 3) acceptor. Varying the length of the n-alkyl chain provided an assessment of molecular chain flexibility. Coated and uncoated aluminum surfaces were characterized by receding water contact angle and surface roughness. Ice adhesion shear strength was determined in the Adverse Environment Rotor Test Stand facility from -16 to -8°C that simulated aircraft in-flight icing conditions within the FAR Part 25/29 Appendix C icing envelope. Surface roughness of the coatings was similar allowing for comparison of the test results. An adhesion reduction factor, based on the ice adhesion shear strength data with respect to uncoated aluminum obtained at the same temperature, was calculated to compare the data. The results revealed complex interactions with impacting supercooled water droplets that were interdependent upon ice accretion temperature, surface energy characteristics of water and ice, hydrogen bonding characteristic of the substituent, and length of the n-alkyl chain. To aid in explaining the results, 1) changes in the surface energy component (i.e., non-polar and polar) values that water undergoes during its’ phase change from liquid to solid that arise from the freezing of impacting supercooled water droplets on the surface depended upon the temperature during accretion were taken into account and 2) the physical properties (i.e., water solubility and melting point) of small compounds analogous to the substituted n-alkyldimethylalkoxysilanes used in this study were compared.

Smith, Joseph G.↗
NASA NTRSDate not supplied

A Statistical Analysis of Impact Ice Adhesion Strength Data Acquired with a Modified Lap Joint Test

Numerous methodologies have been utilized to measure the adhesion strength of impact ice, and the data reported in the literature varies significantly from method to method. In order to initiate an investigation to determine the cause of this disparity, a lap-joint shear test methodology that was recently developed was utilized in the Icing Research Tunnel at the NASA Glenn Research Center. Data was obtained while varying the temperature, test section velocity, liquid water content, and cloud droplet median volumetric diameter, among other parameters, over five campaigns. A new data set acquired using this new test method is presented. The results are analyzed with standard statistical methodologies and demonstrate a strong correlation between the apparent adhesion strength of ice and temperature, annealing time, and heating time. Observations during the test and analysis of the results suggest the presence of large residual stresses in the samples, which is in agreement with prior work. Due to the nature of the test methodology, and all known ice adhesion test methodologies, the measured, or apparent, adhesion strength is geometry dependent, a fact emphasized by the results presented here. The data was organized both cumulatively and independently by result code. Trends in the data are discussed in the context of causal physical mechanisms. The data shows the apparent adhesion strength was not linear with temperature, liquid water content, annealing time, and other variables. Short-term heating of the samples was shown to have negligible effect, and the apparent adhesion strength had a flat trend with velocity.

Ice Adhesion↗
NASA NTRS1997

Tests of the Performance of Coatings for Low Ice Adhesion

This paper reports studies of the performance of low-ice-adhesion coatings by NASA Lewis and BFGoodrich. Studies used impact ice accreted both in the NASA Lewis Icing Research Tunnel (IRT) and in the BFGoodrich Icing Wind Tunnel (IWT) and static ice in a BFGoodrich bench-top parallel-plate shear rig. Early tests at NASA Lewis involved simple qualitative evaluations of the ease of removing impact ice from a surface. Coated surfaces were compared with uncoated ones. Some of the coatings were tested again with static ice at BFGoodrich to obtain quantitative measurements. Later, methods to establish the adhesion force on surfaces subjected to impact ice were explored at Lewis. This paper describes the various test programs and the results of testing some of the coatings looked at over the past 5 years. None of the coatings were found to be truly ice-phobic; however, the most effective coatings were found to reduce the adhesion of ice to about 1/2 that of an uncoated aluminum sample.

Anderson, David N.↗
NASA NTRS2020

Durability Characterization of Low Ice Adhesion and Impact Resistance Coatings

Glaze, rime and mixed icing conditions can cause significant variation in aerodynamic performance, fuel efficiency, and flight safety. For commercial aircraft, active icing mitigation strategies are utilized to enable safe flight within icing conditions according to the FAR Part 25/29 Appendix C icing envelope. For general aviation and unmanned aerial vehicles that cannot support active anti-icing technologies, avoidance is the only recourse. Passive approaches have been investigated to reduce weight and energy consumption for active systems and to expand the operational envelope for smaller aircraft. Coatings are one passive method to reduce or mitigate ice accretion on frontal surfaces of commercial aircraft with the greatest region of interest being wing leading edges. Aircraft wing leading edges represent an extreme environment. Durability must be considered for any material to be applied as a coating in this area. Currently, there are no specifications regarding coating durability of a low ice adhesion material applied on the wing leading edge. Therefore, a reasonable starting point is to use the durability specifications put forth for an aircraft external coating. Besides the tests called out in these specifications, others were included such as Taber abrasion to simulate wear and erosion. Beyond durability, performance metrics with regards to adhesion strength of accreted in-flight (i.e., impact) icing are central to determine coating usefulness. Determination of this property though is particularly challenging and only a few facilities have the capability to quantify this. An instrument at NASA Langley Research Center [Adverse Environment Rotary Test Stand Jr., (AERTS Jr.)], based on the AERTS system at The Pennsylvania State University, allows for screening numerous coatings subjected to the icing environment. To establish a benchmark for comparison with research coatings, a state-of-the-art (SOA) commercial aircraft coating was subjected to an array of salient durability and performance experiments. The same tests were conducted using a baseline epoxy (BE) resin formulation that demonstrated some initial promising results for comparison. Results from this initial screening will be discussed herein.

Miranda L Beaudry↗
NASA NTRS2019

NASA Workshop on Low Ice Adhesion Materials

The first NASA Workshop on Low Ice Adhesion Materials was held on Thursday, August 10, 2017, at the Ohio Aerospace Institute in Cleveland, Ohio. This meeting allowed government, industry, and academia to meet in a collaborative environment to discuss the future of “icephobics” research for inflight icing. NASA presented its ongoing research, and organizations that currently have partnerships with NASA presented their recent findings. Presenters from academia included Iowa State University, Mississippi State University, Pennsylvania State University, and the University of Michigan. Presenters from industry included United Technologies Aerospace Systems; Nanosonic, Inc.; and NEI Corporation. Researchers from NASA Glenn Research Center, NASA Langley Research Center, and the Office of Naval Research also shared their current research. There were over 60 participants who attended the conference plus more than 10 who participated remotely. The meeting was highly successful, and although a second such conference was proposed, it is anticipated that future technical presentations on the subject(s) will take place in other venues. Presentations from this workshop that are suitable for public release are included in this document. This effort supports both the Advanced Air Transport Technology (AATT) Project and the Revolutionary Vertical Lift Technology (RVLT) Project.

Kreeger, Richard E.↗
NASA NTRS2019

Reinforcing Additives for Ice Adhesion Reduction Coatings

Adhesion of contaminants has been identified as a ubiquitous issue for aeronautic exterior surfaces. In-flight icing is particularly hazardous for all aircraft and can be experienced throughout the year under the appropriate environmental conditions. On larger vehicles, the accretion of ice could result in loss of lift, engine failure, and potentially loss of vehicle and life were it not for active deicing or anti-icing equipment. Smaller vehicles though cannot support the mass and mechanical complexity of active ice mitigating systems and thus must rely upon passive approaches or avoid icing conditions altogether. One approach that may be applicable to all aircraft is the use of coatings. Durability remains an issue and has prevented realization of coatings for leading edge contamination mitigation. In this work, epoxy coatings were generated as a passive approach for ice adhesion mitigation and methods to improve durability were evaluated. Highly cross-linked epoxy systems can be extremely rigid, which could have deleterious consequences regarding application as a leading edge coating. Incorporation of flexible species, such as poly(ethylene glycol) may improve coating toughness.8 Additionally, core-shell rubber (CSR) particles have been utilized to improve fracture toughness of epoxies.9 Both of these more established additives are investigated in this work. An emerging additive that is also evaluated here is holey graphene. This nanomaterial possesses many of the advantageous properties of graphene (excellent mechanical properties, thermal and electrical conductivity, large surface area, etc.) while also exhibiting behaviors associated with flexible, porous materials (i.e., compressibility, increased permeation, etc.). Holey graphene, HG, was synthesized by the oxidation of defect-rich sites on graphene sheets through controlled thermal expo-sure.10 It is envisioned that the porous nature of HG would allow resin penetration through the graphitic plane, resulting in better interfacial interaction and therefore better translation of the nanomaterial’s properties to the surrounding matrix.

Wohl, Christopher J↗
NASA NTRS2015

The Effect of Surface Chemical Functionality Upon Ice Adhesion

In nature, anti-freeze proteins present in fish utilize specific organic functionalities to disrupt ice crystal formation and propagation. Based on these structures, surfaces with controlled chemical functionality and chain length were evaluated both experimentally and computationally to assess the effect of both parameters in mitigating ice formation. Linear aliphatic dimethylethoxysilanes terminated with methyl or hydroxyl groups were prepared, characterized, and used to coat aluminum. The effect upon icing using a microdroplet freezing apparatus and the Adverse Environment Rotor Test Stand found hydroxyl-terminated materials exhibited a greater propensity for ice formation and adhesion. Molecular dynamics simulations of a silica substrate bearing functionalized species of similar composition were brought into contact with a pre-equilibrated ice crystal. Several parameters including chain mobility were monitored to ascertain the size of a quasi-liquid layer. The studies suggested that chain mobility affected the interface between ice and the surface more than terminal group chemical composition.

Smith, Joseph G., Jr.↗
NASA NTRS1939

Adhesion of Ice in Its Relation to the De-icing of Airplanes

The various possible means of preventing ice adhesion on airplane surfaces are critically reviewed. Results are presented of tests of the adhesives forces between ice and various solid and liquid forces. It is concluded that the de-icing of airplane wings by heat from engine exhaust shows sufficient promise to warrant full-scale tests. For propellers, at least, and possibly for certain small areas such as windshields, radio masts, etc. the use of de-icing or adhesion-preventing liquids will provide the best means of protection.

Rothrick, A M↗