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Contents lists available at ScienceDirect

**Surface & Coatings Technology
**

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

**Investigation of surface properties and mechanical and tribological
**

behaviors of polyimide based composite coatings

Camelia Demian a,⁎, Hanlin Liao a, Remy Lachat b, Sophie Costil a

a

b

**Laboratoire IRTES-LERMPS, Université de Technologie de Belfort-Montbéliard, 90010 Belfort Cedex, France
**

Laboratoire IRTES-M3M, Université de Technologie de Belfort-Montbéliard, 90010 Belfort Cedex, France

a r t i c l e

i n f o

Article history:

Received 17 June 2012

Accepted in revised form 19 August 2013

Available online 29 August 2013

Keywords:

Polyimide based composite coatings

Total surface energy

Friction coefﬁcient

Wear rate

Thermal stability

a b s t r a c t

This article focuses on the development and characterization of thermoset polyimide (PI) based composite coatings on aluminum substrates. In order to improve the tribological behavior, PTFE and SiC ﬁllers were added into

pure PI to develop composite coatings. A thermal study to validate the condition of the pure PI coating after the

elaboration process was performed using DSC analyses and the Tg evolution with the temperature of a pure

polyimide sample was investigated.

Then, the inﬂuence of the ﬁllers (PTFE and SiC) on surface properties, and mechanical and tribological behaviors

of the PI composite coatings is considered. Results showed that, by adding PTFE particles into the pure PI, lower

surface energies and lower and stable friction coefﬁcients can be obtained. Besides, the addition of SiC particles

improved the mechanical behavior such as hardness and wear resistance of the composite PI–PTFE–SiC coatings.

Following the obtained results, correlations between wear rate depending on total surface energy and

microhardness were established. Thermogravimetric analysis (TGA) of the PI and PI composite coatings was

carried out. The results revealed that the addition of ﬁllers into PI pure matrix improved the thermal stability

of the composite coatings.

© 2013 Elsevier B.V. All rights reserved.

1. Introduction

Advanced composites exhibit appropriate physical and chemical

properties that include light weight characteristics coupled with high

stiffness and strength, dimensional and thermal stability, chemical

resistance, ﬂexural performance and relatively easy processing. The

resin systems used to manufacture advanced composites concern

two basic types: thermosetting and thermoplastic polymers. Thermosetting resins such as epoxy, polyurethane, phenolic and amino, and

bismaleimide (BMI, polyimide) are widely used in advanced composite

manufacturing. As a thermoset polymer, polyimide (PI) possesses

outstanding properties such as excellent mechanical and electrical

insulating properties, good thermal stability and chemical inertness,

high wear resistance and resistance to radiation which make it suitable

for a wide range of applications [1]. In spite of the good characteristics of

polyimide, studies have been carried out to improve their surface properties and tribological behavior by dispersing different ﬁller materials

throughout the polymer matrix. Thus, the PI based composite becomes

a promising material with controlled mechanical or tribological properties. Besides, ﬁllers contribute to optimize the operational properties in

different applications, such as microelectronics or biomedical devices,

components for electrical, aerospace or automotive industries [2–4].

⁎ Corresponding author at: Laboratoire SPCTS, UMR CNRS 7315, Université de Limoges,

12 rue Atlantis, 87068 Limoges Cedex, France. Tel.: +33 0 5 87 50 24 03.

E-mail address: camelia.demian@unilim.fr (C. Demian).

0257-8972/$ – see front matter © 2013 Elsevier B.V. All rights reserved.

http://dx.doi.org/10.1016/j.surfcoat.2013.08.032

Polyimide is also known as a thermo-stable polymer due to its excellent properties at elevated temperatures (250 and 350 °C). The thermal

properties of different synthesized polyimides were already studied by

many researchers. For example, high glass transition temperature of

polyimide up to 310–315 °C [5,6] or 340 °C [7] and no melting point

[5–8] have been observed on different DSC curves. The excellent thermal stability of polyimide from ambient temperature up to 350 °C [9]

or 420 °C [6] has been also reported. Moreover, the polyimide has a

degradation temperature above 500 °C [5,6].

Polymer based composites reinforced at micro or nanoscale with different ﬁllers such as ﬁbers or solid lubricates have gained development

and become promising bulk or coating materials for tribological applications. The mechanical properties of the glass–epoxy composites can be

improved with the addition of SiC ﬁller and this composite presents a

lower wear rate [10]. The addition of the SiC particles in the polymer

matrix as a secondary ﬁller along with graphite into glass–epoxy matrix

increases the wear resistance of the composite material [11]. Like many

kinds of polymer materials, the PI based composite coatings were also

studied. For example, the PI resins ﬁlled with solid lubricants such as

graphite, MoS2 and PTFE particles and reinforced with carbon ﬁbers

(CF) have shown better friction and anti-wear behavior under waterlubrication rather than dry sliding [1]. The addition of appropriate content

of Al2O3 nanoparticles into PI improved signiﬁcantly the tribological behavior [12] of the specimens prepared by compression molding method.

Besides, the tribological properties of polyimide based composites

demonstrated good friction behavior and improved wear resistance

/ Surface & Coatings Technology 235 (2013) 603–610 Fig. either acting abrasively or adhesively for sintered PI composites [14]. desolventation and thermal characteristics. Polyimide P84 solution is presented in the NEP (N-ethyl-pyrrolidone) Glass transition temperature Tg (OC) 350 300 250 200 150 100 150 200 250 300 350 400 450 Isothermal holding (OC) Fig. By the addition of graphite as internal lubricant into pure polyimide.% into a polyimide fully imidized P84 solution (provided by Evonik Industries. lower friction coefﬁcients can be obtained under high loads and high sliding velocities [15]. For this purpose different PTFE weight concentrations as well as a ﬁx amount of SiC particles were incorporated into a fully imidized polyimide resin matrix to fabricate composite coatings. polyimide based composite coatings also offer high surface thermal stability when used in tribological applications. Coating elaboration and characterization methods 2. Besides. if they are ﬁlled with carbon nanotubes (CNT) and Al2O3 [12. DSC curve of the PI coatings. The aim of this study is to investigate the mechanical and tribological behaviors of PI–PTFE and PI−PTFE–SiC composite coatings under dry condition. It is already demonstrated that PTFE signiﬁcantly improved the performances of other polymers such as PEEK [17] and PI [18] because it controls the friction and wear behaviors. 1. 3. Composite coating elaboration PTFE particles with an average diameter of 30 μm were added in 20. increasing SiC whisker content in a SiC–AlN– polyimide matrix composite increased the toughness and decreased the ﬂexural modulus [16]. The use of polyimide based composites as surface protection can improve the tribological behavior and surface properties of different substrate materials. . Fig. SiC particles as a solid ﬁller also contribute to enhance the mechanical and tribological properties of PI based composites.1. Microscopic observations of the coating surface and cross-section were performed in order to reveal the surface morphology. even at elevated temperatures.604 C. few information about the mechanical and tribological behaviors of polyimide composite coatings ﬁlled with PTFE and SiC was reported in the literature. For example. aluminum is widely used in industrial applications for diverse parts and devices. Demian et al. 2. Austria) and well mixed. but it possesses poor friction properties. The results of microhardness and tribological tests were correlated with the total surface energy determined by sessile drop method. Evolution of Tg with temperature. The DSC and TGA analyses were performed on the polyimide solution and pure polyimide and its composite coatings in order to determine the structure after the heat treatment as well as the phenomena which occur during the polymer heating such as glass transition.13]. Besides. However. 30 and 40 wt. 2. The graphite additives can control the interfacial sliding conditions. Evonik Fibres GmbH. Moreover. Surface morphology of PI–20% PTFE–5% SiC composite coating before polishing.

2 4. Coating morphology was investigated using a JSM 5800 LV. Japan scanning electron microscope. B) PI–20% PTFE–5% SiC.C. Demian et al. the coatings were dried in a forced-air furnace at 80 °C for a few hours to evaporate the solvent. The counterpart consisted of a 6 mm diameter 100C6 steel ball with a mirror ﬁnished surface (Ra = 0. which were embedded in epoxy resin under vacuum. The volume loss of the coating was determined by multiplying the cross-section area by the perimeter of the wear track. proﬁlometry traces were taken across the wear tracks generated on the coating surface after tribological test. The sample was embedded in an aluminum pan in the case of DSC analysis and then heated until 500 °C at a heating rate of 10 °C/min. Following the same experimental protocol. Austria. mechanical properties in terms of hardness were determined.3 0.% SiC particles having an average diameter of 1. the perimeter of the circular track (mm): l = 2 × 3. The friction force was measured with a linear variable differential transformer sensor and dynamically recorded into a computer. 4. Then.5 13. To determine the wear rate. The thermal study of the pure PI coating aims to validate the condition of the coating after the elaboration process.142 × r (mm). The wear rate was calculated as: V A l mm3 ¼ w¼ d F d F Nm ! ð1Þ where. The sample surfaces used to evaluate the tribological properties of the coatings and surface energy were polished to reach an average surface roughness between 1 and 3 μm.1.8 9. Friction tests were accomplished using a ball-on-disk CSM tribometer (CSM Instruments. The friction coefﬁcients of the composite coatings were determined by tribological tests using the pin-on-disk method at ambient temperature. and then heated up to 315 °C with a heating rate of 1.9 1. JEOL. The friction coefﬁcients were obtained when the measured forces were divided by the applied load. France). using a 3D AltiSurf 500 proﬁlometer (Altimet. At least 8 indentations using a load of 10 g were performed on the metallographic samples in cross-section using a Leica VMHT 30A Vickers tester.1 7.1 1. the sliding distance (m).2.6 0. were performed according to an adapted procedure using a SiO2 solution for polishing.01 0. The data were recorded using dedicated Universal AnalysisV4 acquisition software. 5 wt. Thermal investigations of the PI coating. provided by Evonik Industries GmbH. 3. solvent.7 μm were added into the PI–PTFE mixture as the second solid ﬁller. PI solution and PI based composite coatings were carried out using differential scanning calorimetry (DSC) and thermal gravimetric (TGA) measurements. to have a clear interpretation of the measures the average and the standard deviation of the results were calculated.6 ± ± ± ± ± ± ± 3 7 2 8 3 7 7 ± ± ± ± ± ± ± 0. Then.5 °C/min to remove the residual solvent and to stabilize the properties of the composite material. The grinding and polishing processes of metallographic samples. 2.03 5. V D F A L the volume loss (mm3). The surface properties were evaluated using sessile drop method to determine the wettability and surface energies according to Owen– Wendt theory [19]. Characterization methods Several investigation methods were used to observe the inﬂuence of ﬁller particles on the surface characteristics and mechanical and Table 1 Coating thicknesses and surface roughness measurements. The microscopic observations in cross-section view have been performed using a Leica DMRM optical microscope. Results and discussion 3.02 μm) and a hardness of 62 HRC. PI based composite coating microstructures: A) PI–20% PTFE. the PI based composite coatings were also analyzed by a series of TGA tests. where r (mm) represents the radius of the wear track. Thermal study of the polyimide matrix The PI matrix is a fully imidized solution containing 25% of polyimide and 75% of NEP solvent. Swiss). 605 tribological behaviors of the composite coatings. / Surface & Coatings Technology 235 (2013) 603–610 Fig. From DSC tests conducted .2 11. the chosen amount of SiC particles is almost the limit in order to favor the application on the Al substrate. The resulting composite mixtures were then applied on Al plates of 50 × 50 × 3 mm to ﬁnally obtain a coating thickness between 60 and 120 μm. The samples were heated until 800 °C at a heating rate of 10 °C/min.3 0. respectively. the applied load (N). These analyses were conducted in air atmosphere using Q10 and Q50 TA Instrument apparatus. which represents 75% of the total mass. Because of the high viscosity of the PI–PTFE mixture. the cross-section area of the wear track (mm2). Coating Thickness (μm) ± SD Roughness Ra (μm) ± SD PI PI–20% PTFE PI–20% PTFE–5% SiC PI–30% PTFE PI–30% PTFE–5% SiC PI–40% PTFE PI–40% PTFE–5% SiC 78 69 63 109 95 120 81 0.0 Finally.

7 60.35 0. 4A).25 PI coating 0. non-wetting occurs if the contact angle θ is higher than 90° and the surface is considered hydrophobic. Friction coefﬁcient of PI and PI based composite coatings depending on sliding distance. The cross-section microstructures of the PI based composite coatings are shown in Fig. a complementary DSC analysis was performed on a PI solution sample.5 29. The total 30 25 HV0. Both thickness and roughness increase with the ﬁller content. In order to detect the position of the Tg on the DSC curve of the PI coating.9 87. associating these results with the DSC curve presented in Fig. Consequently the surface is considered hydrophilic. but a logarithmic trendline cannot be drawn due to point displacements.9 49.7 μm (particle dimensions between 0. 3. For example. Evolution of the surface properties of coatings The measured contact angles and surface energies of the PI and PI based composite coatings are listed in Table 2. and 20 min at 350 °C and 400 °C. For the pure PI coating the water contact angle has a value of 73°. The second exothermal event which could represent the expulsion of the residual solvent enclosed in the polymer molecules is overlapped on the beginning of the degradation process of the polymer.1 83. The addition of SiC particles has a positive effect on the surface roughness for all composite coatings. This process is possible due to the relaxation of the molecular chains during the glass transition phenomenon. When SiC particles are added. 4B).2 28.1 4.0 30. PTFE and SiC particles appear quite homogeneously dispersed into the PI matrix with respect to the different particle diameters: about 30 and 1.5 0. During the heating several isothermal holdings were performed as follows: 150 min at 80 °C.5 29.2 31.2. The composite coating thickness and roughness are listed in Table 1. Vickers microhardness of PI and PI based composite coatings. 80 min at 250 °C and 300 °C.9 72.01 20 15 10 5 Friction coefficient µ 0.05 0 0 200 0 PI PI-40%PTFE-5%SiC PI-40%PTFE Fig. Demian et al. the position of the Tg point of the pure PI coating can be deﬁned around the temperature of 263 °C.3 62. Therefore. It can be observed that the Tg points follow a logarithmic evolution with the temperature increase.1 46.5 25.606 C. Then. The increase of Tg with temperature is due to the solvent expulsion which. As a result.4 35. The PI coating has a very smooth surface with an average roughness Ra of 0. When a mass amount of PTFE above 20% is added. It serves as an indicator of mastery of the coating. an acceleration of heat ﬂow can be observed. v = 0. a homogeneous distribution of the reinforcing agents can be observed (Fig.4 and 6. 1.9 69.1 80.1 PI based composite coatings 0.6 26. the roughness also increases from 5 μm corresponding to the PI–20% PTFE to 9 and 13 μm corresponding to PI–30% PTFE and PI–40% PTFE. the Tg evolution with the temperature is observed.4 29. respectively. θ (°) Total surface energy (mN/m) H2O (water) C2H6O2 (ethylene-glycol) C10H7Br (α-bromonaphthalene) γPs γD s γTs 73. respectively. at high temperatures. Subsequently. 4.7 on a PI solution sample.1 25.7 54. 2 shows the Tg evolution with the temperature.5 μm) for the PTFE and SiC particles.5 97.3. A similar thermal event was observed on the DSC curve of PI ﬁber [6].6 35. Composite coating morphology The composite coatings with different ﬁller concentrations presented similar morphology. Fig.8 42.% PTFE. respectively.0 5.15 0.7 57.0 3. Conversely.4 8. using a fully imidized PI solution no melting point was observed on the DSC curve as shown in Fig.4 33.4 F = 5 N. The addition of SiC particles slightly reduces the thickness and roughness values of the composite coatings ﬁlled with 20. 1.6 41. 30 and 40 wt. 3 presents the surface morphology of PI–20% PTFE–5% SiC coating. Besides. the surface is considered either wetting or hydrophilic. 3. . 1. Besides. Moreover. Several thermal events were observed on the DSC curve of the PI coating presented in Fig. PTFE content does not affect the composite coating morphology (Fig.6 5.1 39. the total surface energy is directly related to the wettability and represents an important parameter which can strongly affect the surface properties.1 41.4 76. 400 600 800 1000 Sliding distance d (m) PI-20%PTFE-5%SiC PI-20%PTFE PI-30%PTFE-5%SiC PI-30%PTFE Fig.5 79. respectively. Material coatings PI PI–20% PTFE PI–20% PTFE–5% SiC PI–30% PTFE PI–30% PTFE–5% SiC PI–40% PTFE PI–40% PTFE–5% SiC Contact angle. The wetting occurs if the contact angle θ between the water droplet and the surface is less than 90°.3 0. A relative homogenous distribution of ﬁllers into PI matrix can be distinguished. The surface roughness considerably increases with the increase of the PTFE particle content in PI matrix. The ﬁrst part of the curve corresponds to the PI heat capacity. 5.8 3.9 98.9 0. 6.0 44. Adding PTFE and SiC reinforcing agents the angle increases up to 98° and the surface becomes hydrophobic for PI– 40% PTFE and PI–40% PTFE–5% SiC coatings.6 54. two exothermic events occur at temperatures of 128 °C and 410 °C. Fig.03 μm compared with the PI based composites. / Surface & Coatings Technology 235 (2013) 603–610 Table 2 Contact angles and total surface energies of PI and PI composite coatings. the composite coating thickness increases from 69 to 109 and 120 μm corresponding to PI–30% PTFE and PI–40% PTFE.6 m/s 0.2 0. acts as a plasticizer.

57 0. the addition of SiC ﬁller leads to a wear rate decrease.17 for the sliding velocities of 0. it can be noticed that the addition of PTFE into the PI matrix leads to a friction coefﬁcient decrease in comparison 607 with the pure PI coating.8 0. the mass loss was much faster and by 700 °C the coating was completely burnt. e.18 0. 8a and b illustrates the linear regression of wear rate depending on total surface energy as well as wear rate depending on microhardness.01 experimental results are listed in Fig.6 0. the proportion of different components in the solidiﬁed coatings should be noted which are displayed in Table 4. PTFE has a lower degradation temperature than the PI.01 0. For example.6.58 mm3/N·m which increases at 2. Accordingly with TGA curves shown in Fig. the degradation process started slowly. On the other side.01 0. The pure PI coating did not lose any signiﬁcant mass.8 m/s were selected to investigate their inﬂuences on the friction coefﬁcients and wear rates.18 0. the wear rate increases along with the PTFE content.6 m/s. the total surface energy also plays an important role. For every test. 3.5. SiC ﬁller was found as a residue but it does not alter the degradation process of the composite coatings.01 0. This difference is highlighted with the increase of PTFE content. The SiC content has less inﬂuence on the total surface energy of the composite coatings.17 0. Along with the increase of PTFE content into the PI matrix.16 0. In general.01 0.52 13.16 for a sliding velocity of 0. Besides.8 0. However.01 0.g.4. 8a.4 0.34 1.4 0.8 0. it is not possible to distinguish the proportion of PI and PTFE which are two organic polymers that degrade in the same temperature range. The real coating compositions were determined by TGA tests. PI coating microhardness reached a value of about 27 HV0.01 0. After that.4 m/s. respectively. The linear regression presented in Fig. From the results listed in Table 3.71 mm3/N·m for sliding velocities of 0.18 and 0. By the addition of SiC particles into the PI–PTFE matrix a slight increase of the friction coefﬁcient can be observed. Fig. / Surface & Coatings Technology 235 (2013) 603–610 Table 3 Friction coefﬁcients at different sliding velocities and an applied load of 5 N as well as a calculated wear rate. For each PI composite coating.4.01 0. the composite coatings have different friction behaviors.6 0.95 1.19 mm3/N·m for the PI–30% PTFE and PI–40% PTFE. The linear regression curve of wear rate depending on total surface energy is illustrated in Fig.6 0.6 0. adding 20 wt.4 0.34 to 0. Generally.17 0. in the case of PI– 20% PTFE matrix.4 and 0. the friction coefﬁcient decreases slightly along with sliding velocity increase but its value varies over a small range.8 0. The wear dependence of PI and PI based composite coatings on sliding velocity is illustrated in Fig. When developing wear protection coatings for tribological applications. Thermogravimetric analysis of the pure PI and PI based composite coatings Thermal stability of PI and PI based composite coatings were evaluated by TGA (Fig.4 m/s and an applied load of 200 N) [18].4 0. Besides.4 and 0.62 0. 6 illustrates the friction coefﬁcient curves of the PI and PI based composite coatings versus sliding distance.71 0.18 0. whose wear rate increases with the sliding velocity increase. The wear rate of PI coating is lower than that of PI–PTFE and PI–PTFE–SiC composite coatings.6 0. Fig. especially for the composite coatings that contain SiC particles.99 1. Sample Sliding velocity v (m/s) Average friction coefﬁcient μ ± SD Wear rate w (mm3/N·m) PI 0. An exception can be noticed in the case of PI coating. The TGA curves show that the composite coatings are more stable than the pure PI coating.34 which is approximately two times higher than that of the PI based composite coatings.4% moisture evaporation occurred at a temperature of 93 °C and then.C. Mechanical behavior The mechanical behavior of the PI and PI based composite coatings was determined by microhardness measurements. 7.34 PI–20% PTFE PI–20% PTFE–5% SiC PI–30% PTFE PI–30% PTFE–5% SiC PI–40% PTFE PI–40% PTFE–5% SiC ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± 0.56 0. respectively. respectively.16 0.6 and 0. Demian et al. If different wt. 0. 9). respectively. Similar friction coefﬁcient of 0.38 0. both wear rate and total surface energy decrease. 8b shows that except the PI coating.01 0. Table 3 illustrates the data input for the friction tests as well as the average friction coefﬁcients obtained for all composite coatings and the calculated wear rates. The addition of PTFE ﬁllers results in a wear rate increase and a surface total energy decrease.6 m/s. The only distinction that is possible to realize is that due to the .6 0. 9.4 0.15 was reported for PI–15% PTFE composite coating.02 4. For example. until about 400 °C.34 0. For example.8 0. the friction coefﬁcients vary in a small range for PI–30% PTFE and PI–40% PTFE. The HV0. with the addition of SiC particles.6 0.67 0. Besides.01 0.17 0.6 and 0. at a sliding velocity of 0. a weight loss of 4% at a temperature of 378 °C. in the case of PI–20% PTFE–5% SiC.08 0. from a wear rate of 0.71 0. other than due to the loss of moisture or the residual solvent expulsion.99 and 4.01 0.19 2.01 which is higher than that of the PI based composite coatings (Fig. where adding the SiC particles slightly increases the total surface energy. an amount of 1.% of PTFE in the PI matrix the friction coefﬁcient decreases from 0.16 0. 3.% of PTFE particles are added into the polyimide matrix a signiﬁcant decrease in microhardness of the composite coatings was observed.17 0. The PI–40% PTFE composite coating reaches a maximum wear rate of 14 mm3/N·m for a sliding velocity of 0.56 to 0.01 0.58 0.42 to 0. for all composite coatings the wear rate decreases with the sliding velocity increase.42 0. PI coating has a friction coefﬁcient of 0.4 0. resulting in the degradation of PI based composite coatings.03 2.8 m/s. An exception can be noticed in the case of PI–40% PTFE. for all composite coatings.6 m/s. Above 400 °C.16 0. For the PI based composite coatings.16 0.47 1.01 surface energy decreases with the PTFE content. the ball slides 1000 m on the coating surface. For example.61 0.52 mm3/N·m. 3.15 0. depending on the ﬁller content.8 0. the friction coefﬁcients have the values of 0. the friction coefﬁcient of composite coatings has a relatively stable value from the start of the sliding track. This may be due to the PTFE ﬁller melting point (about 330 °C) which occurs in the same temperature range as the expulsion of solvent.4 0.03 0.16 0. 5). the composite coatings with a relatively high hardness exhibit less wear.15 0.01 0. 5.17 0. but under harder conditions (sliding velocity of 1. adding SiC particles into the PI–PTFE matrix the microhardness of the PI–PTFE–SiC composite coatings slightly increases. Besides.01 0. The proportions found in the coating residues contain a SiC ﬁller. For example.17 0.01 0.60 14.02 0.01 0. and an offset point can be observed at a temperature of 569 °C. Tribological behavior The tribological tests were conducted at room temperature and lab air environment.17 0. For an applied load of 5 N the sliding speeds of 0.01 0. A minor reduction of the total surface energy can be observed in the case of PI– 20% PTFE–5% SiC and PI–30% PTFE–5% SiC. the wear rate of PI–20% PTFE coating has a value of 0. the addition of SiC particles led to a slight decrease of the wear rate from 0.74 0.

a low wear . The addition of SiC ﬁller reduced the wear rate caused by the action of strong cyclical solicitations and kept in the same time the low friction coefﬁcients. Analyzing the results presented in Tables 2 and 3. From the point of view of both friction and wear behaviors. 9) which could correspond to the residual solvent evaporation. the polymer degrades. Moreover.4 0. 8. which could inﬂuence the mechanical properties of the composite coating matrix.6 0. For PI–20% PTFE–5% SiC coating. This is due to the addition of the PTFE ﬁller which is known for its low total surface energy. high concentration of PTFE in the composite coatings the thermal events associated to PI are masked by those associated to PTFE. The total surface energy decreases along with the PTFE content increase from 46 to 26 mN/m2 for PI and PI–40% PTFE coatings. it can be noticed that low total surface energies lead to low friction coefﬁcients. A complete desolventation of the polyimide is hard to accomplish. the wear rate signiﬁcantly decreases in the case of PI–30% PTFE–5% SiC with about 94% in comparison with PI–30% PTFE or with 86% for PI–40% PTFE–5% SiC in comparison with PI–40% PTFE. in the case of a sliding velocity of 0. Wear rate of PI and PI composite coatings depending on sliding velocity.6 0.6 0. Still. but it contains a less solvent amount. Discussion DSC analyses performed on the pure PI coating revealed a high Tg point which along with the TGA results. a mass loss of PI coating was detected on the TGA curve beginning with the temperature of 310 °C (Fig. Moreover.42 mm3/N·m against 14.% SiC particles into the fully imidized PI resin demonstrated an improved mechanical behavior by a slight increase in hardness. The effect of degassing process results in an effective process control for the drying procedure of the PI–PTFE–SiC composite coatings.4 0.4 0. because it is directly related to the temperature and time and with a temperature increase. Concerning the stability of pure PI matrix in the absence of solvent. the wear rate has a low reduction of 8% in comparison with PI–20% PTFE.4 0. b) wear rate depending on microhardness. a decrease of the mechanical properties of the ﬁnal composite coatings.4 0.6 0. the wear rate increases quickly (PTFE presents a low hardness).8 0. the analysis performed on a Wear rate w (mm3/N·m) a 5 4 3 2 1 0 20 Wear rate w (mm3/N·m) b 30 40 50 20 30 Total surface energy γsT (mN/m2) 5 4 3 2 1 0 0 10 HV0.34 to 0. indicate that the PI matrix is thermally stable above 400 °C.02 mm3/N·m for PI–40% PTFE. the addition of 5 wt. PI solution sample demonstrated that the Tg increases with the temperature increase and results in a thermally stable PI at an elevated temperature. an incorrect heat treatment which ended up with a lower Tg could affect the properties of the ﬁnal coatings. e. However when increasing the amount of PTFE ﬁller into the PI matrix.8 Sliding velocity v (m) Fig.16 which corresponds to a sliding speed of 0. respectively.g.6 0. Demian et al.4 0.01 Fig. Consequently.6 m/s for PI and PI–40% PTFE coatings.4 m/s. / Surface & Coatings Technology 235 (2013) 603–610 14 Wear w (mm3/N3m) 12 10 8 6 4 2 0 0. 3. This justiﬁes the main studies concerning the thermal behavior of the pure PI coating. For example. it can be observed that the addition of 20% PTFE and 20% PTFE + 5% SiC into PI matrix has the best behavior in terms of a moderate friction coefﬁcient.8 0.7.8 0. Moreover.8 0. Linear regression curves of PI and PI based composite coatings: a) wear rate depending on total surface energy.4 0. 7.8 0. the wear rate of PI is 0.6 0.608 C.6 0. The PI coating demonstrated a low wear rate because of its high hardness. If the heat treatment of the PI coating is performed at a temperature above 350 °C the polymer could be damaged. along with total surface energy decrease the friction coefﬁcient decreases from 0.

-L. The hardness as well as the wear rate increases with the increase of PTFE amount into the PI–PTFE composite coatings. Technol. a slightly decreased wear rate and a satisfactory hardness in comparison with the other PI–PTFE–SiC composite coatings. [3] C. 68 (2008) 1570–1578. Moreover.%. Moreover.Q. Wu. the addition of PTFE signiﬁcantly contributes to the total surface energy decrease and consequently to the reduction of the friction coefﬁcient of the PI based composite coatings. In addition. the PI–20% PTFE–5% SiC composite coating still presents a low friction coefﬁcient. rate and an acceptable mechanical behavior. K. Sci. PTFE addition has a positive inﬂuence on the surface properties of the PI composite coatings but negative with respect to the mechanical and tribological behaviors in terms of hardness and wear rate of the PI composite coatings. Austria for the polyimide P84 solution supply. W. Table 4 Composition of the PI composite coatings. . By the addition of 5 wt. DSC and TGA investigations of the pure polyimide solution samples and PI and PI based composite coatings were performed. The addition of the SiC particles has no inﬂuence on the surface properties of the PI based composite coatings but signiﬁcantly improves the mechanical and tribological behaviors of the PI–PTFE–SiC composite coatings. A 356 (2003) 48–53. total surface energy and friction coefﬁcient of the composite coatings. PI–20% PTFE–5% SiC composite coating demonstrated a lower total surface energy than the pure PI coating. References [1] J. 4. due to the thermal stability of the matrix. Thus the PI–20% PTFE composite coating revealed a low friction coefﬁcient. Mater. [2] A. the addition of 15 wt. the addition of PTFE and SiC ﬁllers into pure PI matrix thermally stabilizes the PI–PTFE–SiC composite coatings. Conclusions This study proposed to investigate the surface properties as well as the tribological and mechanical behaviors of the PI–PTFE–SiC composite coatings.D. J. Yang. Thereby. Moreover. TGA curves of PI and PI composite coatings. Chen. the PTFE ﬁller considerably decreases the friction coefﬁcient of the PI–PTFE–SiC composite coatings.M. Tanaka. Jia.-K.H. Gao.% of PTFE ﬁller into the pure PI matrix is sufﬁcient to have interesting results with respect to the tribological and mechanical behaviors of the PI based composite coatings. this is also underlined by the thermal stability of SiC and PTFE particles like ﬁllers and their positive inﬂuence on hardness. Sessile drop method investigations revealed that increasing the PTFE amount up to 30 wt. 9. Based on the results obtained with respect to PI composite coating investigations.% the PI composite coatings have a hydrophilic character then a hydrophobic character is noticed for the PI–40% PTFE and PI–40% PTFE–5% SiC. Zhou.C. Increasing the amount of PTFE to 30 and 40 wt.% PTFE and 10 wt. A correlation between the mechanical and tribological behaviors can be noticed.-T. The TGA results showed that the PI coating is thermally stable at an elevated temperature (above 400 °C). several conclusions can be made. Wear 257 (2004) 1096–1102. S. Initial composition of the composite coatings (Before the furnace drying) Final composition of the composite coatings (After the furnace drying) PI–20% PTFE PI–20% PTFE–5% SiC PI–30% PTFE PI–30% PTFE–5% SiC PI–40% PTFE PI–40% PTFE–5% SiC PI–50% PTFE PI–44% PTFE–12% SiC PI–63% PTFE PI–57% PTFE–10% SiC PI–73% PTFE PI–66% PTFE–9% SiC DSC analysis revealed a high Tg point of the pure PI coating.% and adding SiC particles the total surface energy still decreases. The PI–PTFE–SiC composite coatings which demonstrated a good hardness exhibit less wear. Besides. Thus. T. according to TGA results. the Tg of the pure polyimide solution increases with the temperature increase. Acknowledgments The authors are grateful to the company Evonik Industries-Evonik Fibres GmbH.% SiC particles.-B. The calculated total surface energy decreases with the increase of the PTFE wt. Sci. Eng. Chen.12 [18]. Adding 20 wt. especially the effect of PTFE and SiC reinforcing agents. / Surface & Coatings Technology 235 (2013) 603–610 609 Fig. S. Another trend suggested by this study is the possibility to use the PI–PTFE–SiC composite coatings for high temperature applications.% CNT into a PI matrix highly decreased the friction coefﬁcient to 0. C. Umeda. Min. Demian et al. Compos. Under harder dry sliding conditions. H. Takatsu.

Yang. A 364 (2004) 94–100. Arun. Wear 301 (2013) 122–129. K. 23 (6) (1994) 557–564.610 C. Sadananda Rao. P. P. [11] S. [15] P. P. Ghosh. Liu. Yan.D. Chandramohan. Zhang. J. [6] G. J. Appl. [8] M. Zhao. T. [18] S.L. G. Seetharamu. Sci. F.doi. Y. Friction and wear of ﬁber reinforced polyimide composites. Charact. S. [14] P. Schoukens. Polym. P. Demian et al. Reinf. Anal. 43 (8) (2003) 1477–1487. Yijun. Polym. Q. Li. [7] Q. Compos. [19] D. Plast. Paulo Davim. Polym. Thermochim. Mita. R. Electron. B. [12] H. Sen. F. Song. Polym. Wang.S. Yan. Cai.C. Samyn. [17] J. G. Alizadeh. X. Wang. J. 13 (1969) 1741–1747. Polym. Sci.X. Z. Eur. Wear 270 (2010) 57–72. Horie. A 31 (1993) 2345–2351. Q. K. Hendrickx. Bhat. H. R. Yin.PolymSci. 41 (2005) 1097–1107. S. W. R. J. Samyn.J.H. Ghaemy. Hussainova. Sun. Xue. De Baets. Yamashita. Jin. F. I. L. T. Owens. Sci. J. Polym. Cai.2012. M. D. Eng.C.Y. D. Sci. Basavarajappa. http://dx. 45 (2009) 3108–3115.wear. Mater.12. Therm. 26 (6) (2007) 565–578. De Baets. J. Acta 389 (2002) 19–24. Mater. 22 (2003) 875–882. M. R. Bijwe. [13] H. 49 (1997) 399–405. [10] B. G. F. Wang. Y. Suresha.J.019. Chung. [5] S. Sampathkumaran. J. Xue. Wendt. Antonov. Tan. I. Meng.K. Schoukens. S.10 16/j. C. Xiaohua. Shao. Schwanke. Liwen.V. Behmadi. [16] L. S.D. [9] Y. Test. J. J. . X. Eur.R. Q. Eng.org/10. 121 (2011) 1574–1578. Appl. Wang. Eng. Wear 258 (2005) 1536–1542. Xin. 8 (2009) 379–391. / Surface & Coatings Technology 235 (2013) 603–610 [4] G. Mater. Li. Yokota. J. A. Zhao. Miner.

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