Dental Materials (2004) 20, 947955

www.intl.elsevierhealth.com/journals/dema

Effect of ber position and orientation on fracture load of ber-reinforced composite

Scott R. Dyera,b,*, Lippo V.J. Lassilab, Mikko Jokinenb, Pekka K. Vallittub
a

Department of Restorative Dentistry, Division of Biomaterials and Biomechanics, Division of Prosthodontics, School of Dentistry, Oregon Health and Science University, 611 SW Campus Drive, Portland, OR 97239, USA b Department of Prosthetic Dentistry and Biomaterials Research, Institute of Dentistry, University of Turku, Turku, Finland
Received 12 March 2003; received in revised form 21 November 2003; accepted 23 December 2003

KEYWORDS
Dental material; Composite resin; Fiber; Fiber position; Fiber orientation; Fracture; Deection; Failure mode; Initial failure; Final failure

Summary Objectives. The aim of this study was to determine the effect of ber position and orientation on the initial and nal fracture loads of ber-reinforced composite (FRC). Methods. Test specimens made of two indirect particulate composites (BelleGlass HP, Kerr, Orange, CA) or (Targis, Ivoclar Vivadent, Amherst, NY) were reinforced with ultra high molecular weight polyethylene (UHMWPE) ber ribbon (Connect, Kerr, Orange, CA), woven E-glass bers (Vectris Frame, Ivoclar Vivadent, Amherst, NY) or unidirectional R-glass bers (Vectris Pontic, Ivoclar Vivadent, Amherst, NY). Fibers were placed with different positions, orientations or geometry into the rhombic test specimens (2 2 25 mm3). Control specimens did not contain ber reinforcement. The test specimens n 6 were stored in distilled water for 1 week at 37 8C before testing in a three-point loading test to determine the initial and nal fracture load values. Results. Initial failure loads varied from 22.6 to 172.1 N. The lowest value resulted from one UHMWPE reinforcement ber located in diagonal orientation and the highest from two unidirectional glass ber reinforcements, one located on the tension side and the second on the compression side. Signicance. Position and ber orientation inuenced the load to initial and nal failure, and specimen deection. Tension side reinforcement was most effective in increasing the load to initial and nal fracture. Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction
*Corresponding author. Address: Department of Restorative Dentistry, Division of Biomaterials and Biomechanics, Division of Prosthodontics, School of Dentistry, Oregon Health and Science University, 611 SW Campus Drive, Portland, OR 97239, USA. Tel.: 1-503-494-8335; fax: 1-503-494-8260. E-mail address: dyers@ohsu.edu

Composite materials are a combination of two or more distinct components forming a new material with enhanced properties. While many combinations exist, the most common composites in engineering are composed of strong bers held by

0109-5641/$ - see front matter Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.dental.2003.12.003

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a binder or matrix. Unlike traditional materials, the properties of composites can be designed simultaneously with structural aspects. This allows composite designers to manipulate material properties by changing ber orientation, ber content, and geometry. Additionally, the most common types of matrix materials are polymers [1]. Attempts have been made to reinforce dental polymers with several types of bers for various treatment modalities during the past 30 years. Studies have tested polyethylene bers [2], carbon/ graphite bers [3 5], or glass bers [6 9]. There exist potential applications for ber-reinforced composites (FRC) in prosthodontics, periodontics, and orthodontics. Several in vitro studies have been conducted to nd out and understand the factors inuencing dental FRC properties [10 15]. Important factors inuencing the mechanical properties of FRCs include: (1) inherent material properties of bers and polymer matrices, (2) ber surface treatment (sizing) and impregnation of bers with resin, (3) adhesion of bers to the polymer matrix, (4) quantity of bers [16], (5) direction of bers, (6) position of bers [17 19] and (7) water sorption of FRC matrix [16]. Previous dental FRC research on position and orientation has focused upon the effects of the question of ber reinforcement directionality (i.e. random or longitudinal orientations) [20,21]. It is widely accepted that directional orientation of the ber long axis perpendicular to an applied force will result in strength reinforcement. Forces that are parallel to the long axis of the bers, however, produce matrix-dominated failures and consequently yield little actual reinforcement. Design strategies are on occasion employed to provide multi-directional reinforcement, to minimize the highly anisotropic behavior of unidirectional ber reinforcement. Multidirectional reinforcement, however, is accompanied by a decrease in strength in any one direction when compared with unidirectional ber, as described by Krenchel [22]. In most instances in the dental literature, ber reinforcement has been positioned in the center of a composite specimen [20]. Yet from engineering applications, it is known that the position and orientation of the reinforcement within a construction inuences mechanical properties [23]. For a small sized construction, such as a dental prosthesis, the quality and characteristics of the FRC are important and demand careful attention. Fiber reinforcement should be optimal when designing prostheses and their components. As an example, the components (e.g. connector, pontic, retainer) of a FRC xed partial denture (FPD) need to be designed to withstand masticatory loading [24].

While it is known that tension side ber reinforcement strengthens a loaded construction, the effect of varying the cross-sectional design in a FRC structure is not fully known. Respectively, all factors relating to design and failure of FRC structures should be investigated and better understood. Questions exist whether ultra high molecular weight polyethylene (UHMWPE) bers can be used to fabricate a high quality dental composite structure. Criticism has been focused on ndings that interfacial adhesion between polyethylene bers and dental polymers is not adequate [25,26]. The use of resin pre-impregnated silanized glass bers instead of non-impregnated polyethylene bers results in the highest mechanical properties according to the majority of recent research [27,28]. A subtle and under-reported attribute of FRC is a description of the fracture failure. A specimen may catastrophically fail in an instant while another may simply bend under increasing load. In 1975, Craig and Courtney described three modes of failure that can occur when characterizing FRC in a tension type test [29]. The three failure modes are described as instantaneous (Fig. 1, Curve A), statistical (Fig. 1, Curve B), and stepwise (Fig. 1, Curve C). Instantaneous failure occurs after a load causes a strain concentration in a narrow region sufcient to break the composite structure. A strain concentration distributed to a wide region may require further load or elongation for continued fracture. Thus leading to what is denoted as stepwise (more bending type) or statistical failure (series of small intense fractures which recover before complete failure and require more load to progress). Analysis

Figure 1 Graphical examples of tension test failure modes of unidirectional glass FRC. Curve A is described as instantaneous failure, curve B as statistical failure (series of small intense fractures which are prevented from becoming catastrophic), and curve C as stepwise failure (more bending type). Note the designation of the knee or corner and areas of unstable condition of the stress-strain curve.

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Table 1 Description of materials used in the investigation. Materials used (from manufacturers information) Name BelleGlass HP Connect Connect resin Targis Vectris frame Vectris Pontic General composition Methacrylate ester monomer/BisGMA/TEGDMA particulate composite (78% ller: Ba-Silicate, SiO2) Gas plasma treated woven polyethylene (reactive methacrylate ester monomers) Methacrylate ester monomer/Bis-GMA/TEGDMA particulate composite (74% ller: Ba-Silicate, SiO2) Bis-GMA/UDMA/DDMA particulate composite (80% ller: Ba-Silicate, SiO2) Woven E-glass (50% weight). Bis-GMA/UDMA/DDMA/TEGDMA matrix (5% ller: SiO2) Unidirectional R-glass (65% weight). BisGMA/UDMA/DDMA/TEGDMA matrix (3.5% ller: SiO2) Batch number 809477 9911065 907626 B06115 A95063 A95049 Manufacturer Kerr/Sybron (Orange, CA) Kerr/Sybron (Orange, CA) Kerr/Sybron (Orange, CA) Ivoclar Vivadent (Amherst, NY) Ivoclar Vivadent (Amherst, NY) Ivoclar Vivadent (Amherst, NY)

BISGMA 2,2-bis[4-(2-hydroxy-3-methacrylyl-oxyporpoxy)phenyl]propane; DDMA decandiol dimethacrylate; TEGDMA triethyleneglycol-dimethacrylate; UDMA urethane dimethacrylate.

of the mode of failure can give insight on how and why failure occurs. Accurate reporting should therefore include when the fracture begins (initial fracture), how it progresses, and when it nishes (nal fracture) [30]. The aim of this study was to compare the effect of various positions, orientations, and geometries of glass and polyethylene bers in a dental particulate composite test specimen upon the initial and nal fracture load. It was hypothesized that there would be no difference in load to failure among designed specimen groups.

Materials and methods

The materials used in the study are given in Table 1. Rhombic test specimens (2 2 25 mm3) were made in a three-piece stainless steel mold. Three main groups of specimen were categorized according to the type of ber used in each test bar. Specimens were fabricated according to selected cross-sectional designs as shown in Fig. 2. Test groups (n 6/group) consisted of a cross-sectional design of specic ber reinforcement. Specimens in the main group, PE ( polyethylene ber-reinforced composite), consisted of the par-

ticulate composite Belleglass HP (Kerr, Orange, CA) and the cold gas plasma treated ultra high molecular weight polyethylene (UHMWPE) reinforcement Connect (Kerr, Orange, CA). The UHMWPE ribbon was hand impregnated with the light curing resin, Connect Resin (Kerr, Orange, CA). The UHMWPE braided weave (two over/two under) was dispensed to a length of 25 mm from a 2 mm wide spool and classied as one unit of ber reinforcement (weight accepted 0.0092 ^ 0.0002 g). Group PE received 2 min of visible light cure followed by a post cure of 138 8C for 20 min. Specimen group, W (woven E-glass ber-reinforced composite), contained the particulate composite Targis and Vectris Frame (Ivoclar Vivadent, Amherst, NY), a preimpregnated woven E-glass (electrical glass). A 2 0.4 25 mm 3 section (weight accepted 0.0412 ^ 0.0002 g) was cut from the preformed woven ber (one under/three over). The specimens were light cured for 2 min with a post cure in a visible light cure chamber (Targis Power, Ivoclar/Vivadent, Amherst, NY) for 20 min. Specimen group U (unidirectional ber-reinforced composite) denote test specimens made of the particulate composite Targis and Vectris Pontic (Ivoclar/Vivadent, Amherst, NY), a preimpregnated unidirectional R-glass. The

Figure 2 An example of the derivation of the cross-sectional pictogram. Object A is a three-dimensional depiction of the specimen with ber reinforcement (B) in the center of the long axis of the rhombic bar. The resulting pictogram (C) is the representation of the cross-sectional design of the specimen.

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unidirectional ber was cut to 25 mm length and separated into weighed increments (0.068 ^ 0.002 g), designating one ber reinforcement group. Specimens in group U were cured according to the method described for group W. Cross sections were designed to test possible structural formulations of ber position and orientation. Seven simple cross-sectional designs such as bers positioned on the compression or tension side were used in all three main groups. More complex designs were created with the ber reinforcement as practical within each group (2 5 complex designs in each main group). The threedimensional cross-sectional designs were converted into two-dimensional pictograms like the example in Fig. 2 for ease of description and are presented in Tables 1 3. The ber positions are depicted as solid black lines within the square outline of the specimen. The specimens were

fabricated with the three-piece metal mold upon a clean glass slide and separating sheet. The particulate composite and ber reinforcement were hand incorporated with special attention to form the desired design without void inclusions. Another clear plastic matrix was placed on top of the mold with a clean glass slide and the initial 2 min light cure was initiated. Specimens were carefully released from the metal fabrication mold. Only specimens with dimensions of 2.0 mm (^ 0.1 mm) 2.0 mm (^ 0.1 mm) 25 mm (^ 1.0 mm) were accepted. Five of the 204 specimens were rejected due to heights greater than 2.1 mm. Those specimens were fabricated again and the resulting dimensions were within the acceptable range. Fiber weight and volume percent were calculated and veried with an ashen test [10] with mechanical removal of the ceramic particulate llers.

Table 2 Report of ber weight % and volume % and the deection in mm at initial failure (IF) and nal failure (FF) with the failure mode description (by %) for UHMWPE designs. The specimen names correspond with the adjacent cross-sectional design pictorial (lines within depict where the corresponding ber was placed). Superscript letters denote groups not statistically different ( p , 0.001) for each test. Bar type: PE NF 1 Diag 1 TF 1 MF 1 MPF 1 BF 2 Perp 2 Para 8 Perp 8 Para 3 Para 3 Perp 3 Z Bar I (5) BAR 20.5 46.5 12.3 28.0 39.7 75.8 8.2 18.6 Symbol Fiber weight % 0 4.1 Fiber volume % 0 9.3 Mean initial failure deection in mm (S.D.) 0.48 (0.08)A,B 0.46 (0.04)A,B 0.43 (0.07)A,B 0.47 (0.11)B,C 0.39 (0.035)A 0.62 (0.89)A,B,C 0.78 (0.17)B,C 0.47 (0.51)A,B 2.2 (0.49)E 2.3 (0.24)E 0.52 (0.65)A,B 0.93 (0.10)C 1.3 (0.26)D 2.1 (0.15)E Mean nal failure deection in mm (S.D.) 0.48 (0.08)X 3.0 (0.40)Y 0.43 (0.07)X 3.3 (2.3)Y 2.7 (0.26)X 2.0 (0.27)X,Y 1.5 (0.30)X,Y 2.6 (0.11)Y 2.2 (0.49)X,Y 2.3 (0.24)Y 2.8 (0.36)Y 2.7 (0.55)Y 3.1 (0.89)Y 2.7 (0.64)Y Failure mode % (instantaneous/ stepwise/statistical) (100/0/0) (16.7/33.3/50) (100/0/0) (33.3/0/66.7) (0/0/100) (0/33.3/66.7) (16.7/33.3/50) (0/0/100) (0/100/0) (0/100/0) (0/66.7/33.3) (0/33.3/66.7) (0/33.3/66.7) (33.3/67.7/0)

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Table 3 Report of ber weight % and volume % and the deection in mm at initial failure (IF) and nal failure (FF) with the failure mode description (by %) for woven E-glass designs. The specimen names correspond with the adjacent cross-sectional design pictorial (lines within depict where the corresponding ber was placed). The specimen W (4) @ Comp denotes that four increments of woven e-glass surround the particulate composite. Superscript letters denote groups not statistically different ( p , 0.001) for each test. Bar type: W Symbol Fiber Fiber Mean initial failure Mean nal failure Failure mode % (instantaneous/ weight % volume % deection in mm (S.D.) deection in mm (S.D.) stepwise/statistical) 0 9.2 0 8.1 0.63 (0.18)A,B,C 0.42 (0.15)A,B 0.37 (0.09)A 0.44 (0.06)A,B 0.82 (0.15)C 18.4 16.2 0.88 (0.20)C 0.69 (0.12)B,C 47.7 44.1 1.2 (0.17)D 1.2 (0.11)D 36 32.4 0.80 (0.19)C 0.63 (0.18)W,X,Y 0.42 (0.15)W 0.85 (0.55)W,X,Y 0.57 (0.16)W,X 1.0 (0.31)Y,Z 0.90 (0.20)X,Y 0.79 (0.13)W,X,Y 1.4 (0.13)Z 1.5 (0.09)Z 1.4 (0.10)Z (100/0/0) (100/0/0) (50/0/50) (33.3/50/16.7) (66.7/16.7/16.7) (100/0/0) (66.7/16.7/16.7) (16.7/83.3/0) (0/100/0) (50/ 16.7/33.3)

NF 1 TF 1 MF 1 MPF 1 BF 2 Perp 2 Para 5 Perp 5 Para W (4) @ Comp

All specimens were stored at 37 8C in distilled water for 1 week [31]. The three-point bending test was conducted according to the ISO 10477 (test span: 20 mm, cross-head speed: 1.0 mm/min, indenter: 2 mm diameter) with the specimen wet directly from the storage container. All samples were loaded in material testing machine (model LRX, Lloyd Instruments Ltd, Fareham, England) and the load-deection curves were recorded with PC-computer software (Nexygen, Lloyd Instruments Ltd, Fareham, England). The beginning of the specimen damage formation was classied as the initial failure (IF). IF was denoted if at least two of the following conditions were present, (1) a sharp decline in the load/displacement curve, called a knee or corner [23], (2) visible signs of fracture [23], (3) audible emissions, caused by the generation of elastic waves by crack formation and/or progression [23, 30,32]. The nal failure (FF) of the specimen was characterized as one of the following: (1) attainment of an instability condition, dened as a zero (or negative) slope of applied stress verses strain [30], or (2) the maximal load or displacement before the load decreased by 50% or an apparent catastrophic rupture. The fracture mode was

determined after testing following Craig and Courtneys descriptions [29]. Means and standard deviations were calculated and reported. ANOVA and the post hoc test Tukeys multiple comparison test were used to determine the signicance of the data within ber groups for IF, FF, deection at IF, and deection at FF (Winks, TexaSoft, Cedar Hill, TX).

Results
The mean load required to cause IF of UHMWPE ber-reinforced test specimen varied from 22.6 to 108.0 N and from 33.1 to 108.8 N for FF (Fig. 3, Panel A). Table 2 shows the mean deection of UHMWPE reinforced test specimens at IF and FF, statistical groupings, weight and volume percents, and description of the fracture mode by percent of specimen. The mean load to IF of woven glass berreinforced test specimens varied from 23.7 to 166.0 N and for FF from 24.6 to 166.7 N (Fig. 3, Panel B). Table 3 shows the mean deection of the woven E-glass reinforced test specimen at IF and FF, statistical groupings, weight and volume percents,

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Figure 3 Graphic representations of the load to initial and nal failure (in Newtons) of various cross-sectional FRC designs. The pictorial cross-sectional symbols depict the design of ber incorporation and correspond with Tables 2 4. Letters within the graphs denote specimen groups that are statistically not different ( p , 0.001) for test. The y-bars represent standard deviations. Panel A shows the results for UHMWPE, panel B for woven E-glass, and panel C for unidirectional R-glass.

and description of the fracture mode by percent of specimen. The highest load for the initial and nal failure (172.1 and 184.0 N, respectively) was found with specimens reinforced with unidirectional glass

bers (Fig. 3, Panel C). The mean deection at IF was lowest with unidirectional glass bers in the compression side of the specimen at 0.322 mm (Table 4). Statistical analysis with ANOVA revealed

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Table 4 Report of ber weight % and volume % and the deection in mm at initial failure (IF) and nal failure (FF) with the failure mode description (by %) for unidirectional R-glass designs. The specimen names correspond with the adjacent cross-sectional design pictorial (lines within depict where the corresponding ber was placed). The specimen U (2) @ Comp denotes 2 units of unidirectional glass surrounding the particulate composite, Comp @ Uni (1) denotes 1 unit of unidirectional ber centered in a specimen of particulate composite, and W (4) @ Uni (1) denotes that four increments of woven e-glass surround 1 unit of unidirectional reinforcement. Superscript letters denote groups not statistically different ( p , 0.001) for each test. Bar type: U Symbol Fiber weight % 0 19.7 Fiber volume % 0 17.4 Mean initial failure deection in mm 0.63 (0.18)A,B,C 0.32 (0.05)A 0.45 (0.08)A 0.62 (0.16)A,B 2.0 (0.33)E 39.4 34.8 0.90 (0.08)B,C 0.90 (0.09)B,C 60.7 39.4 19.4 59.2 57.3 34.8 17.4 52.2 0.93 (0.04)C 0.92 (0.12)B,C 0.43 (0.13)A 1.4 (0.22)D Mean nal failure deection in mm (S.D.) 0.63 (0.18)V 0.32 (0.06)V 4.1 (0.27)Z 1.6 (0.10)W 3.4 (4.3)Y 1.8 (0.80)W 1.8 (0.23)W 2.3 (0.25)W,X 2.2 (0.25)W,X 2.7 (0.32)X,Y 2.12 (0.55)W,X Failure mode % (instantaneous/ stepwise/statistical) (100/0/0) (100/0/0) (0/16.7/83.3) (16.7/0/83.3) (0/83.3/16.7) (16.7/50/33.3) (0/16.7/83.3) (0/100/0) (0/100/0) (0/0/100) (16.7/83.3/0)

NF 1 TF 1 MF 1 MPF 1 BF 2 Perp 2 Para 4 Fiber U (2)@ Comp Comp @ U(1) Woven (4) @ Uni (1)

that ber position and orientation signicantly affected the initial and nal failure loads ( p , 0.001). Results of the post hoc analysis are given within the graphs in Fig. 3 and in Tables 2 4 (letters denote groups that are not statistically different).

Discussion
This study demonstrated the inuence of positioning of various types of bers on the fracture load of FRC test specimens. Principally, a similar test setup was used when Vallittu in 1993 reported that position change of metal reinforcement made no signicant difference on the strength of denture base polymer. That result was likely attributed to poor interfacial adhesion between metal and the denture base polymer. Positioning of unidirectional E-glass ber in the same study did show signicant effect on strength and modulus of elasticity of FRC materials 33]. In this study, more complicated cross

sectional designs of ber/matrix structures were tested. Describing the FRC failure with fracture indicators and mode characterization may provide needed insight into composite structure design. Fracture mode and IF have not been previously analyzed in regards to dental FRC. Reporting elastic limit and ultimate strength undoubtedly has its their place in materials science. The question, however, of what did the ber reinforcement actually accomplish, is answered in part by describing the changes in the IF, FF, and fracture mode. There was no difference between an ultimate strength value and initial failure for certain specimens (e.g. unreinforced controls and other experimental reinforced designs) because the failure mode was instantaneous. There was clear distinction between IF and FF for other specimens (e.g. PE groups 3 Para, 1 MF and U group 1 MF). Reporting solely the ultimate strength of such specimens ignores the fracture process that began at a much lower load. Damage and failure initiation, before permanent deformation, may induce or

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accelerate undesirable effects. For example, water ingress will reduce the service and lifetime of the structure [1]. Initial failure may consequently be a more sensitive or useful an indicator than ultimate strength for in vitro strength evaluation and possible clinical interpretation. Regarding composite design principles for continuous reinforcement, placement of ber in regions other than the tension side showed no signicant increase in the load to IF. This is in agreement with early studies [18,19]. The specimen IF agreed with the ndings that in failure the performance of FRCs is regarded as ber or matrix dominated, which evolved from the observation that failure is dominated by one of the composite constituents, not usually a combination of both [34]. This experiment essentially demonstrated that IF performance was dominated by the particulate or ber-reinforced composite. While FRC materials have the ability to slow or arrest crack propagation, fatigue and hygrothermal corrosion may advance the crack to complete or partial failure (e.g. delamination) [34]. The ber reinforcement minimized the instantaneous and catastrophic failures while additionally retaining specimen fragments. Greater load was needed to advance the fracture process for the majority of designs. The design considerations of a composite construction would need to address performance criteria of elevating the required load to initial failure or simply maintaining component fragments after fracture. An example of the effect of ber conguration orientation can be seen when comparing the load to IF of PE groups 3 Para, 3 Perp, 3 Z bar. In many cases, a simple change in ber orientation statistically affected the load to failure. The use of eight UHMWPE bers in the bar 8 Perp, creating a laminate composite, resulted in lower load to IF than the geometrical design of ve ber groups in the I (5) bar. Such design characteristics may be possibly employed in prosthetic components. Two of the FRC materials used in this study were in an unpolymerized pre-preg form (woven and unidirectional glass bers) and one was wetted with polymer resin at the time of specimen assembly. The overall fabrication technique, however, is classied as a hand lay up process. The hand lay up process is typically subject to more errors in FRC fabrication than other techniques such as pultrusion or bag transfer molding [1]. In the case of these dental FRC specimens the seven common designs required relatively minimal effort of fabrication. The complex FRC designs increased the technical difculty and time (approximately ve times) required for fabrication. Of the complex crosssectional designs in all three main groups, only two

of the complex UHMWPE designs (3 Z bar and I (5) bar) had signicantly higher loads to initial failure that the simple designs. Scanning electron microscopy has shown good adhesion between glass ber and matrix along with relatively poor adhesion between UHMWPE and matrix resins [25]. An effect of this may be evident in the PE bar 1 Diag, which had a lower load to IF than the control, though not signicantly. Regardless, UHMWPE tension side reinforcement increased the load to IF by 60%, while complex UHMWPE geometry raised the load to IF by a 220% increase. Unidirectional glass ber appears to reinforce the test specimen when even partially positioned at the tension side (group U, 1 MPF and 2 Para). Increased exural rigidity of the specimen may also contribute increased load to failure. Further investigation is required to delineate between the contributions of increased stiffness and tension side reinforcement. While more sophisticated equipment is becoming prevalent for acoustic emission analysis [32], the use of audible emission, even without amplication,1 provided verication of IF with the stress strain curve knee. Investigations in composite structures, notably FRC, not recording or reporting damage initiation and accumulation are omitting valuable data. The methodology used in this investigation limits interpretation to statically loaded rhombic test specimens. Fatigue loading complex specimen designs could address questions more closely related to masticatory loading in the oral environment.

Acknowledgements
This study was nancially supported the Finnish Technology Agency (TEKES). A portion of the work was conducted under the NASA/Texas Space Consortium 2002-2003 Fellowship. Materials were supplied by the manufacturers, which is greatly appreciated.

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