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This content was downloaded from IP address 152.66.184.111 on 22/10/2024 at 09:23 Nanotechnology Nanotechnology 35 (2024) 435201 (12pp) https://doi.org/10.1088/1361-6528/ad66d3 Implementation of microcontroller board on a sustainable and degradable PLA/flax composite substrate: a case study Attila Géczy1,2,∗, Dániel Piffkó1, Richárd Berényi1, Karel Dusek2, Pascal Xavier3 and David Cuartielles4 1 Department of Electronics Technology, Faculty of Electronic Engineering and Informatics, Budapest University of Technology and Economics, Budapest, Hungary 2 Department of Electrotechnology, Faculty of Electrical Engineering, Czech Technical University in Prague, Prague, Czech Republic 3 IMEP LAHC, University Grenoble Alpes, Universite´Savoie Mont-Blanc, CNRS, 38000 Grenoble, France 4 Arduino Verkstad AB, Malmö 211 77, Sweden E-mail: geczy.attila@vik.bme.hu Received 19 February 2024, revised 24 June 2024 Accepted for publication 23 July 2024 Published 5 August 2024 Abstract In this paper, we present a novel polylactic-acid/flax-composite substrate and the implementation of a demonstrator: a microcontroller board based on commercial design. The substrate is developed for printed circuit board (PCB) applications. The pre-preg is biodegradable, reinforced, and flame-retarded. The novel material was developed to counter the increasing amount of e-waste and to improve the sustainability of the microelectronics sector. The motivation was to present a working circuit in commercial complexity that can be implemented on a rigid substrate made of natural, bio-based materials with a structure very similar to the widely used Flame Retardant Class 4 (FR4) substrate at an early technological readiness level (2–3). The circuit design is based on the Arduino Nano open-source microcontroller board design so that the demonstration could be programmable and easy to fit into education, IoT applications, and embedded designs. During the work, the design was optimized at the level of layout. The copper-clad pre-preg was then prepared and processed with subtractive printed wiring technology and through hole plating. The traditional surface mounting methodology was applied for assembly. The resulting yield of PCB production was around 50%. Signal analysis was successful with analogue data acquisition (voltage) and low-frequency (4 kHz) tests, indistinguishable from sample FR4 boards. Eventually, the samples were subjected to highly accelerated stress test (HAST). HAST tests revealed limitations compared to traditional FR4 printed circuit materials. After six cycles, the weight loss was around 30% in the case of PLA/Flax, and as three-point bending tests showed, the possible ultimate strength (25 MPa at a flexural state) was reduced by 80%. Finally, the sustainability ∗ Author to whom any correspondence should be addressed. Original content from this work may be used under the terms of the Creative Commons Attribution 4.0 licence. Any further distribution of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI. 1 © 2024 The Author(s). Published by IOP Publishing Ltd Nanotechnology 35 (2024) 435201 A Géczy et al aspect was assessed, where we found that ∼95 vol% and ∼90 wt% of the traditional substrate can be substituted, significantly easing the load of waste on the environment. Keywords: biodegradable, PCB, commercial electronics, educational electronics, Arduino Nano, PLA composite, single-board microcontroller 1. Introduction Larguech et al [12] performed thermal and dielectric analysis on PLA/PBS (polybutylene succinate) blend matrix after jute fibre reinforcement. At low temperatures, dielectric permittivity was improved after reinforcement of the blend matrix. The study by Kumar and Gupta [13] compared classical Flame Retardant Class 4 (FR4) with jute and epoxy, sisal and epoxy, and hemp and epoxy-based potential composite materials. The results showed that the combination of epoxy and jute, sisal, or hemp has almost the same properties as classical FR4. However, the authors did not address the issue of flame retardancy, which is a critical aspect of natural-based fibres. Ryan-Fogarty et al [7] proposed a new composite material for PCB fabrication by recycling methods to recover components from PLA boards. The process successfully separated the electronic components, copper bands, glass fibres and polylactic-acid. However, glass fibre is a weak point as long as it requires separate treatment during recycling and cannot be composted. Bharath et al [14] proposed the incorporation of banana fabric as reinforcement, but their work did not show more advanced application case studies. Yedrissov et al [15] demonstrated PCB manufacturing from recycled and renewable materials, where various components were recovered during the process. Sudheshwar et al [16, 17] have proposed paper-based electronics with additive patterning. Arroyos et al [18] produced a prototype computer mouse consisting of a biodegradable PCB, a compostable PVA case, and a limited set of electronic components. The applied Soluboard PCBs and the PVA case were dissolved in water, and after disassembly, many of the components could be reused. However, from a commercial point of view, solubility seems to be a limiting factor, and water is a central point of reliability issues related to assemblies [19]. In our previous studies, we successfully produced PLA and CA-based RFID cards in different sizes Kovács et al [20], and a media player as a commercial application was presented. Fibre reinforcement and solder mask applicability was lacking, and the assemblies presented were very sensitive to conventional reflow (reflow soldering) temperatures, even with Sn–Bi-based solder alloys at reduced melting point (138 ◦ C). We improved this with the introduction of the PLA/Flax composite with flame retardancy, which showed promise in biodegradability of the carrier substrate, application in surfacemounted technology (SMT), sustainability, reliability, and the missing parameters, namely fibre reinforcement and flame retardancy [21]. Electronic devices are an essential part of our modern and evolving world; the number of circuits is constantly growing due to the ever-increasing demand. The lifetime of these circuits, however, is not unlimited. At the end of their life cycle, most electronic devices end as hazardous waste. The amount of e-waste is around 60 million tonnes annually and is projected to increase by 2 million tonnes annually [1, 2]. Asia has the highest e-waste production, while Europe has the highest e-waste per capital. Approximately 10% of waste is diverted, mostly illegally, to poor developing countries to recycle valuable metals that can be recovered from e-waste back into the trade [3]. However, exposure to highly toxic substances and untimely and unskilled work processes can shorten the lives of people involved by decades [4]. The Brundtland Report [5], published by the United Nations in 1987, defines sustainable development as ‘development that meets the needs of the present without compromising the ability of future generations to meet their own needs.’ According to the strict sustainability model, increasing economic capital can only be at the expense of natural capital, which cannot be increased and includes economic and social capital, as these are part of our environment as subsets of it. The current electronics industry cannot be sustained in the long term, as our raw materials resources and waste storage capacity are finite. From this aspect, one possible point of easing the load on the environment and resources is to find alternative technologies and materials in electronics, such as focusing on packaging materials. In recent studies (Khrustalev et al) [6], it was found that about 70 wt% of the waste printed circuit board (PCB) generated is glass fibre reinforced epoxy composites, which are difficult to process and harmful to the environment if left in e-waste piles. Metals can be recovered from the composites by hydrometallurgical, mechanical, or pyromechanical treatment—also problematic regarding environmental impact (Ryan et al) [7]. Thus, many focus on this aspect in their studies. The development of sustainable electronics is mainly based on polylactic acid (PLA) substrates. This use has been investigated from several perspectives in recent years (Schramm et al [8], Mattana et al [9], Henning et al [10], Hong et al) [11]. However, many studies have omitted flame retardancy and fibre reinforcement (even more, the combination of the two), leading to more reliable assemblies. 2 Nanotechnology 35 (2024) 435201 A Géczy et al Figure 1. The cross section of the substrate presents the structure (thicker inner textile, refined outer textile) and through-hole vias (with fibre-based burrs). According to the findings above, we focus on the following in our current research. We wanted to validate our novel substrate promoting degradability with a feasible and straightforward application of current technologies and features. The current paper presents the implementation of a small footprint controller board on a sustainable PLA/Flax composite biodegradable substrate, starting from surface mounting assembly to actual tests of the microcontroller board. The presented complexity (to be discussed later) is intended to be higher than what we could obtain from the literature. The exemplary application also promotes sustainability, where the expected reduction of actual wt% of generated e-waste [7] is above 70% with completely degradable substrates. With the application of an Ardunio Nano microcontroller board [22], we choose an example where commercial complexity could be achieved with a widely used circuit (released under Creative Commons Attribution Share Alike 3.0 License). The PCB substrate is a result of a collaboration between BME-ETT and Meshlin Composites Zrt [21]. 2.2. Experimental steps The following experimental was set to present the research implementing the commercial complexity circuitry on the sustainable bio-substrates. The mind map of the experiment is presented in figure 2. First, the analysis and optimization of the adopted circuit design were considered in CAD software to avoid errors, which could arise from previously investigated material parameters, such as surface roughness [21]. We used the original files. While we are not at the technical readiness level (TRL) of the technology to have exact design rules for our technology limitations, we tried to polish the design, so that any possible failures would be minimized. The full documentation, schematic and layout design can be accessed at [25]. Afterward, subtractive PCB technology was used to prepare double sided printed wiring on traditional FR4 and PLA/Flax boards. The copper clad was processed with photolitography and copper etching processes. The technology steps are using plated through-holes (Dow chemicals and Crimson direct electroplating) and selective chemical surface finish (ImAg, immersion silver, ∼0,5 µm thickness) according to the technology steps of our laboratory [26]. It has to be noted, that the plating of through hole is aimed for 25 µm thickness, which adds up to the copper thickness on the top and bottom layers (∼60 µm thickness altogether). This, and the evenness of top/bottom layers, and the unevenness of the through hole platings can be also seen in figure 1. Finally, traditional photosensitive solder mask is printed (SunChemicals, Imagecure, XV501T) to improve soldering of surface mounted components, albeit reducing the degradablenon degradable ratio of applied materials. The mask is finished with 150 ◦ C/60 min baking process. Laser-cut (Coherent Avia UV Nd:YAG) stencil (100 µm thick) was used for stencil printing with low-temperature Sn42/Bi57.6/Ag0.4 (no-clean, T4 type, melting point: 138 ◦ C) Tin–Bismuth solder alloy (Chipquik, SMDLTLFP60T4). 2. Experimental 2.1. Biodegradable substrate The structural design of the substrate and the common FR4 composite are similar but mainly differ in the materials used. The FR4 substrate is a glass fibre-reinforced epoxy resin composite with flame retardants. In the case of the degradable substrate used, the glass fibre is replaced by a set of flax fibre textile fabric (grammage between ∼200–300 g m−2 ), and the epoxy resin is replaced by polylactic acid, presented in powder and foil form. The novel composite is flame retarded with natural retardants. The current application improved upon previously published versions using linseed oil to reduce water absorption possibility, which was found to be a problem in initial experiments [21]. Figure 1 presents a cross-sectional view of the degradable composite, showing the structure of the substrate and the materials used. In table 1 we have added a summary of available and comparable (with FR4) material parameters according to their practical unit highlights in given literature. 3 Nanotechnology 35 (2024) 435201 A Géczy et al Table 1. Parameter comparison. Parameter, unit PLA/Flax [21, 22] FR4 [23, 24] Dielectric Thickness, mm Starting copper Thickness, µm Effective Permittivity @ 2–2.4 GHz Loss Tangent @ 2–2.4 GHz Peel strength, N/mm Flame-retardancy Tg, ◦ C Thermal Diffusivity, cm2/s 1,6 (see figure 2.) 35 ∼2.3 ± 0,1 (2,4 GHz) ∼0,04 ± 0,01 (2,4 GHz) ∼0,6–0,8 UL94 V0, EN 13 501–1 ∼60–100 0.000 565 1,6 (variable) 35 (variable) 3,93 (2 GHz) 0.0167 (2 GHz) 1,19–1,6 UL94 V0 170 0.0027 Figure 2. Mind map of the experimental—from goal to finish (CAM rework, PCB substrate fabrication, SMT assembly, yield analysis, functional tests, HAST, and mechanical tests. Manual component placement was performed on the boards. With programmed profiles, the soldering was performed for both sample types in a computer-controlled, laboratory bench-top infrared-oven (Eurocircuit, ec-Reflow-Mate) suitable for prototyping. The oven is working in laboratory air environment, and was found to be suitable for controlled low-temperature settings and experimenting at early TRL. Through-hole soldering was performed with hot iron soldering (Bakon 938 hand soldering station, operated at 300 ◦ C) after validating more drastic point-like heating on the boards. Figure 3 presents the reflow profiles considered for measurement set in the Eurocircuits oven software. The primary considerations for the profile settings were to minimise the time and to set the maximum temperature as low as possible. Also, the most critical component (ATMEGA168P-20MU, QFN; 500 µm pitch with 230 µm pads) had to be joined succesfully. To quantify the effect of applied temperature profiles, heating factors (Qη) were calculated [27]. The following equation is used to determine the heating factor (1): tˆ A,B,C (T (t) − TX ) dt Qη = (1) t0 where Qη is the heating factor [s◦ C], practically the effect of temperature in time on the board, T(t) is the measured temperature, Tx is the boundary temperature (usually the liquidus of the solder), t0 to tA is the time window from entering and passing the boundary temperature during heating and cooling [s]. The cooling was performed on natural ambient convection after finishing with the profiles. 4 Nanotechnology 35 (2024) 435201 A Géczy et al Figure 3. Programmed temperature profiles applied for soldering. The soldering was performed with IR-based reflow heating. Table 2. Main design rules and final board parameters defined for The cross-section (X-cut) of samples was prepared with an ATA Saphir 520 wet grinder. For optical inspection, Olympus BX51 microscopes were used with Olympus DP72 cameras; for non-destructive x-ray analysis, Nordson Dage Quadra 5 microscope was used. For contact measurements, a Gossen Metrawatt METRA HIT 30 M-type multimeter was used. The short-tests and x-ray analysis revealed the validity of plated through holes too, while cracks or delaminations in similar environmentally friendly substrate materials [28] can cause hidden problems around these features. The technological steps can be seen in greater details in [26], starting from a copper-clad laminate for two-sided boards with through-hole vias. The bootloader is a fixed background code that controls the controller and allows the device to be programmed easily from the ArduinoIDE interface. An official Arduino Nano microcontroller was used for programming. A simple interstitial circuit was developed for this step that connects the corresponding legs of the microcontrollers. The defined sample programs were written to test the digital and analogue voltage output, analogue voltage input (data acquisition), and serial communication over USB. For these tests, a program reads the voltage of a 1000 µF capacitor connected to its input, slowly losing its charge through a resistor, causing its voltage to decrease over time. With one pin configured as an output, the microcontroller recharges the capacitor for 1 s at a given time step. We connected an LED to a PWM-compatible output leg to optically test working, where LED brightness gradually decreased as the capacitor slowly discharged. Testing was extended with signal generation analysis (sinusoidal, 4 kHz) reading and eventual processing in Matlab. Finally, highly accelerated stress test (HAST) extreme environmental load analysis was applied. This test method exposes the tested circuits to the most extreme environmental parameters. We used Espec, EHS-211 HAST chamber in the test, with unassembled circuits. The carriers were exposed to extreme conditions for a total of 6 d. The condition of the circuits was checked daily. The total weight of the PLA/Flax and control FR4 substrates was documented. The cycle parameters were set to a minimum temperature of 105 ◦ C and 100% humidity. The chamber automatically sets the required pressure to achieve the desired temperature and humidity. The pressure value for the set parameters was 120% of atmospheric pressure. The weight data of the examined boards the layout. Design rule/Parameter, unit Value Number of copper layers Copper trace width (min), mm (mil) Copper to copper, mm (mil) Edge keepout, mm Minimum component pitch, mm Minimum via diameter, mm Number of Vias Number of Signal lines Longest signal line, mm Number of Pads Size of the board, mm 2 (top and bottom) 0.254 (10 mil) 0.203 (8 mil) 0.4 mm 0.5 mm 0.5 mm 41 43 82.85 125 43.2 × 18 were registered with a Radwag PS 210. R2 precision laboratory scale (Radom, Poland) with 10 µg certified precision, 1 µg readability, and repeatability in the ambient environment. After HAST, 1–1 degradable and FR4 control samples and two degradable and two FR4 treated samples were sent for 3-point bending (Zwick Roell, DIN EN ISO 14125). The aim was to visualize and quantify the extent to which the structure of the substrates used in the experiment had weakened during the HAST cycle. 2.3. Case study of design optimization It was important to minimize via count and irregular shapes in the design to minimize possible failures during production. While we experimented with designs involving SOIC-8 (with 1.27 mm, 50 mil pitch) before [21], our current QFP package has 500 µm pitch and 230 µm wide pads, which requires ∼10 mil trace width. So small copper fills with related vias were removed. The original 0.2 mm edge keepout was increased from the board outline to avoid delamination (0.4 mm). The minimum trace width was increased to 10 mil (∼0.254 mm), and the copper to copper was kept at 8 mil (∼0.203 mm). The main parameters are presented in table 2 All trace-via connections were corrected to a regular 90 ± 45◦ angle to reduce possibility of improper etching. Corner holes were switched to fiducial points to aid stencil alignment. Silk and solder mask layers were also further 5 Nanotechnology 35 (2024) 435201 A Géczy et al Figure 5. FR4 control sample (top) and PLA/Flax sample (down). Figure 6. Non-wetting solder balls on contact pads caused by excess linseed oil precipitations. All FR4 boards were found to be without errors by optical inspections (as expected). During the inspection under the microscope following the soldering, no short circuits, tears, or other soldering defects were found on the FR4 samples. Figure 5 presents the samples as a comparison between the two assemblies. The degradable composite, laminated with copper foil on both sides, was produced as a sheet measuring approximately 30 × 40 cm. Examination of the substrate surface showed that the copper layer is slightly inhomogeneous, with minor surface voids observed, similar to the findings reported in [21]. Small oil spots were observed on the surface of the degradable composite. The state of the linseed oil on the substrate was characterised as solid. Warming and wiping, petrol cleaning, or upholstery cleaning spray did not remove the oil stains; however, we could remove the surface contamination with acetone. The linseed oil could be removed from the surface by rubbing the circuit’s surface with a lint-free wipe soaked in acetone. During initial tests, we observed solder non-wetting (figure 6) on several pads without cleaning. Wiping ceased these issues. Figure 4. (a)–(b) Reduction of small copper fills and vias; (c)–(d.) FR4 and PLA/flax representation of (b.)—practically identical results; (e)–(f); simplification of intricate silk-screen layer; (g)–(h) FR4 and PLA/flax representation of (f.)—practically identical results. optimised to avoid precision screen positioning requirements. Examples are seen in following figure 4. 3. Results 3.1. Production results Initially, ten pieces of boards were produced from FR4 and PLA/Flax. Samples were prepared with the same assembly manners (with traditional SAC305 Sn–Ag–Cu type solder alloy and higher soldering temperatures). Both technologies were evaluated according to the experimental plans. 6 Nanotechnology 35 (2024) 435201 A Géczy et al Figure 7. Short failures on various x-ray images; comprehensive x-ray image of the circuit (top); short between D13 and GND (bottom left); short between RST and GND (bottom right). Table 3. Yield analysis of the produced batch. No. of board Observation Short (pin-pin) Consideration 1 2 3 4 5 6 Heavy contamination of linseed oil, excess shorting. Clear surface Miniscule spots of contamination Heavy contamination of oil, a few contaminated vias Clear surface Miniscule spots of contamination X Workable Workable Workable Workable X 7 Clear surface 8 9 10 Miniscule spots of contamination Heavy contamination, pad lifting Clear surface D11-D12; GND-RST-A4-AA5-A6-A7-5 V GND-D13 — — GND-RST GND-D3-D11-D13 D9-D10 GND-RX0-VIN A5-A6-A7 A3-A6 GND-RST GND-RST-D11-D13 Cross-section analysis (shown in figure 1) on the PLA/Flax samples revealed that the through-holes have uneven surfaces at the plating, which reduces the internal diameter of the vias. The reinforcement causes this issue. During the currentless hole metallization process, a layer of metal is deposited on the wall of the hole with remaining burrs observed. This effect did not cause any problems during assembly. Nevertheless, the results are promising at this TRL level— no similar board with effectively formed hole metallization has yet been characterised in the literature. Our contact tests showed that all vias performed without a failure over the number of boards, even when small spots of linseed oil residues remained in the holes. Further short circuit tests, however, revealed further failures of production. In 8 of the 10 circuits tested, short circuits were found; in 4 circuits, we found more than one short circuit. The exact location of the short circuits could not be determined with an optical microscope. X-ray photographs of the short circuits found were taken for documentation and to assist in rework. (x-ray is later also used after surface mounting). X Workable X X In one rendered image, both sides (top and bottom) plus the through hole vias are visible for failure detection. Open circuits are also practical to detect with the contrast of the x-ray images. We followed this step by mechanically brushing off the located short circuits. After the correction steps, there was no metallic contact between the previously contacting nets. Figure 7 presents a set of shorts revealed by x-ray imaging, and later, the obtained pictures also helped yield analysis (table 3). The initial explanation for the existence of short circuits was thought to be the short etch time of copper, which was set to the standard FR4-based processes. However, the xray contrast should show a gradual thickness change; the substrates examined had one or at most two short circuits. If these were due to the shortness of the etch time, it is unlikely that we would experience so few and so distinguishable short-circuit locations, while at other points in the circuit, the copper patterns of the different conductors are well separated, and there is a high contrast ratio between the conductor-insulator. Also, a clear correlation between board cleanliness and shorts could not be established. (As seen in table 1). 7 Nanotechnology 35 (2024) 435201 A Géczy et al Figure 8. Assembled circuit on PLA/Flax with pin rows. It was concluded that vertical mask alignment issues due to surface unevenness during subtractive printed wiring technology could cause the shorts, which could be eliminated by using more prominent features in patterning or reducing the surface roughness of the boards [21]. We know, that the average roughness depth (Ra) were 5.77 µm and the average peak to valley height (Rz) of the dielectric surace were ∼16 µm according to ASME B46.1 and ISO 4287 standards [21] of or PLA/Flax boards. These larger vales are due to occasional peaks and valleys in the composite. In case of FR4, the Ra is below 1 µm [29], the latter parameter is slightly more 1 µm [30]. Reducing the roughness is a serious task of the future. By optimizing the layer structure at the top and bottom of the dielectric, and improving the copper-to-dielectric interface will result in a more evenly surface, and reduced maskmisalignment issues. Summing up, the initial yield was 50% with rework and post-processing, which aligns with the technological maturity expected at this basic research stage. Table 3 contains the summary of the yield analysis. The pins are defined in the original documentation of the Arduino Nano circuit [22]. The first two profiles had a more significant impact on the boards. The elevated heating resulted in a slight excess of linseed oil; however, further contamination was avoided using Profile C, and joints generally formed along the boards. With elevated temperatures, a few minor errors were found. In one case, solder wicking was found to cause a short between the leads of the USB connector. Further rework was necessary for the microcontroller package as well for one pin. Such complications arose from minor contaminations from hightemperature oil spills, emphasizing the necessity of low temperature and proper cleaning. However, these are occasional, not consequential issues. Soldering the through-hole pin rows for the board was also performed with hand soldering. The metalized fibrs in the holes caused a slight resistance in pin insertion. The board could withstand efficient hand soldering at 300 ◦ C with SAC alloy at the pins without noticeable damage. The bootloader program was successfully loaded onto the microcontrollers. After soldering and subsequent rework, functional tests followed—at this point, achieving a functioning circuit of this complexity is a major achievement. Figure 8 presents a figure of an assembled board on PLA/Flax circuit. 3.2. Solderability test of degradable circuits 3.3. Basic functional tests of biodegradable substrates Different solder profiles were applied to perform component and board joining (A, B, C as seen in figure 3). The following heating factors were calculated for the different profiles. The first two profiles were programmed to have approximately Qη A : 38 000 [s◦ C] and Qη B : 36 000 [s◦ C], and the third had Qη C : 32 300 [s◦ C], a 15% reduction of heating compared to profile A. From the profile validation measurements (available from the oven software) and calculations according to (1), we found that the actual heating resulted in ∼5% lower Qη values. The actual board temperature could not follow the oven’s transients completely; however, this can be considered a precise follow in reflow technologies. It also has to be noted that the calculations were not related to the usual temperature boundary (solder alloy melting point) but were defined from the starting point to the immediate cooling of the boards to reveal how the total structure was affected by the whole heat applied to the board. The microcontroller’s internal oscillator is working, and this is evident from the success of programming and running basic programs. The question was what the microcontroller perceives from the outside world by detecting analogue signals, without the need to prove high frequency operation, and thorough validation of the dielectric. The sampling frequency of the system is 10 kHz with the analogRead() function. With our calculations according to additional tasks performed by the system, the sampling was found to be 8800 Hz approximately, so we chose a slightly lower value than half of this frequency (4 kHz ultimately). Figure 9 shows the load and discharge of the test capacitor—where the two boards were practically indistinguishable. This proves the practical applicability of the substrate in such scenarios. We used a function generator to connect a signal of known frequency, voltage, and shape to one of the analogue input legs of the microcontroller and sample the signal from the input. From the resulting data, we plotted the frequency composition 8 Nanotechnology 35 (2024) 435201 A Géczy et al the significantly higher degree of degradation of the substrates is immediately apparent. They show delamination of the layers, delamination of the solder resist and assembly markings, oxidation of the copper surfaces, and the appearance of PLA as white porous contamination on the surface of the circuits. Examining the tray on which the substrates were placed in the HAST chamber, it is noticeable that the tray edge (on which the substrates were degraded) was also heavily contaminated. The measurement results also show a reduction in the weight of the degradable substrates (figure 12.). It can be seen that during the cycles, the mass of the carriers decreased monotonically, showing precipitating parts of the composite. The initial minimal increase in mass is due to minimal water absorption by the circuits due to 100% humidity. After six cycles, the weight loss was around 30% in the case of PLA/Flax. The effect of PLA and the linseed oil impregnate loss is validated by the discussed comparisons. The PLA has a density of ∼1,25 g cm−3 , linseed oil has ∼0,9 [31] at given temperature, so the loss of PLA has to be a significant factor in the degradation, even if water moisture is absorbed by the structure. In the case of FR4-based circuits, no heavy degradation was observed optically. Between cycles, oxidised copper surfaces and a slight fading of the green colour of the solder mask were observed. The mass measurements confirm this, since no change was recorded after an initial mass increase. In this case, the results can be seen from both pros and cons. It is clear that the biodegradable substrates will prove with low reliability in a harsh environment. The structure of the novel material limits applicability in extreme environments, but the test also showed that the board will not resist environmental factors during planned degradation, which is a positive outcome. In an ambient environment, such effects will not be observable. The three-point bending test results reveal the changes before and after HAST in figure 13, where the stress-strain curve is shown for the PLA/Flax boards (reference without HAST and two treated samples). The recorded ultimate strength for control sample FR4 was ∼300 MPa, which reduced to ∼200 MPa after the HAST cycles, meaning a ∼33% reduction in the original values. The figure shows the untreated PLA/Flax substrates where ultimate strength presents ∼25 MPa peak, which is much lower than the values of FR4, suggesting weaker mechanical performance for this kind of substrate. This was further reduced to below 5 MPa after HAST (∼80% decrease), meaning HAST has a much higher impact on the degradable boards. Figure 9. Measurements PLA/Flax. Figure 10. Comparison between FR4 (top) and PLA/Flax measurements (bot), 4000 Hz 4Vpp, 2.5 V _off, SIN. of the signal using Matlab’s (Fast Fourier Transform) function. As shown in figure 10, a 4 kHz sinusoidal signal with a peak-to-peak of 4 V and an offset voltage of 2.5 V was applied to the inputs of microcontrollers created on degradable and FR4 substrates. According to the sampling rules, spikes in the frequency spectrum are seen at 3960 and 4896 Hz. (Deviance from optimal 4000 and 4800 Hz is due to the inaccuracies of the utilized ADC in the microcontroller.) It can be seen that the results obtained from the sampling data are practically indistinguishable, regardless of the substrate. We conclude that the analogue circuit tests showed no differences at the given application level. We have verified that operation is practically similar on both PLA/Flax and FR4based Arduino Nano systems; the basic functions work as intended. This analysis is a complementary result to previous findings in [25], where an FPGA functionality at higher speed was investigated on a previous generation of our substrate. 4. Discussion on sustainability According to the final Gerber files of the design containing the copper surface, we determined that the substrate takes ∼95% by volume (vol%) and ∼90% by weight (wt%) of the circuit structure. This means that in FR4-based PCBs, these proportions are associated with the epoxy-glass fibre composite itself, which is complex and not environmentally friendly to process when it becomes e-waste. The studied material completely replaces this composite. These figures indeed point to 3.4. HAST tests on the boards After six days of HAST, comparing the images of the circuits before the first cycle and after the last (6th) cycle (figure 11), 9 Nanotechnology 35 (2024) 435201 A Géczy et al promote SDG 4 (Quality Education). The device could be used in secondary and higher education classrooms as a green electronics demonstrator, targeting a sensitive and receptive audience. 5. Conclusions We presented a successful case study on implementing a microcontroller board on a sustainable PLA/Flax composite biodegradable substrate. We have successfully created a functioning panel on a composite substrate of natural origin and biodegradability with natural fibre reinforcement and flame retardancy. The complexity of the panel is considered to be in line with the commercial level for popular microcontroller boards. We were able to boot an Arduino system and use its functions. Similar circuit was not found in our literature research by traditional subtractive printed wiring patterning and SMD technology with biodegradable substrates. It was found that mask alignment issues and minor surface unevenness caused occasional shorts at the formed copper traces; however, most of the shorts could be reworked. 170 ◦ C IR-based reflow was successful. Another issue was the contamination of the pads caused by the impregnated linseed oil, which was removed with acetone. Later, the further spill was avoided with careful heating, eliminating soldering failures. Higher temperatures are not recommended due to the resulting spill contamination and thermal degradation of cellulosebased reinforcement. PCB production was concluded with a 50% yield. QFNs with 450 µm pitch and 170 µm pads were successfully soldered. Signal analysis was successful with analog voltage reading and low-frequency (4 kHz) signal tests, practically showing equivalent working behaviour with the reference FR4 samples. HAST tests showed precipitations on the boards, showing leaving constituents (such as PLA and oil impregnate). After six cycles, the weight loss was around 30% in the case of PLA/Flax. After the cycles, the possible maximum load (25 MPa at a flexural state) was reduced by 80%, resulting in weak and brittle samples. The extreme ambiance is not suitable for this kind of substrate; however, this also suggests that the boards will degrade in longer-term exposure in proper environment; thus, future recycling of copper and components will be possible. One of the central values of the work from the side of sustainability is that by replacing the traditional FR4-based (fibreglass, epoxy resin) boards with our substrate, about 90% of the volume and mass fraction of the total PCB assembly could be replaced by a sustainable, environmentally friendly, naturally sourced and degradable alternative (the substrate itself), which is a revolutionary change in the e-waste impact of PCBs as we know it today, as repeatedly demonstrated in the literature. As for biodegradability, we have to note that PLA is effectively degradable only in closed and specific environment [32], however flax-based textiles are more generally degradable. The degrading processes should be in line with the requirements of PLA. Also it is important to note, that before actual Figure 11. After HAST analysis. a change in the impact and sustainability of e-waste, and the current results (albeit with only two layers of PCBs) represent an improvement over the ∼70% presented by (Khrustalev et al 2022). According to the current Gerber copper area analysis, it is estimated that the vol% and wt% values (while maintaining PCB thickness) will decrease with increasing the number of copper layers (e.g. 4–6 layers) to 70–80%. According to the UN Sustainability Development Goal points (SDGs) [18], the results point to SDG9 (industry, innovation, and infrastructure), as we are striving for sustainability along all three concepts, with the same production infrastructures as used in current SMT production. In addition, the drastic reduction of e-waste strengthens SDG 12 (responsible consumption and production), further scaling up the attractiveness of the consumer side (‘green electronics’) and the responsible use of raw materials in production, which can have implications for more up to SDGs 13–15. If the Arduino device were to be used for educational purposes, it could also 10 Nanotechnology 35 (2024) 435201 A Géczy et al Figure 12. Weight change after HAST. the possible application will be limited to more general, commercial use. These factors need further investigation, but the results improve upon most similar work in the literature, not focusing on water solubility [17] and maintaining degradability and stability. In future works, we aim to achieve TRL4/TRL5 (TRL4–5 laboratory validated technology, pilot test) implementation of the above concept. The current results were found to be satisfactory at the presented TRL2–3 level. Data availability statement All data that support the findings of this study are included within the article (and any supplementary files). Figure 13. Stress-strain curves of PLA/Flax. Acknowledgments We thank for the help of EFI-Labs in laboratory measurements. Supply of the substrates from Meshlin is highly appreciated. Focus on reflow and heat transfer was partially supported by the National Research, Development and Innovation Office—NKFIH, OTKA Project no. FK 132186. The material and the demonstrator is in focus of of the DESIRE4EU HORIZON-EIC-2023-PATHFINDERCHALLENGES-01-04 Project No. 101161251. degradation process, the components and the conductors could be mechanically separated. Bioleaching is also in our future focus.” In the future, separating copper and components would allow easier recycling of non-degradable components. By using this material, the ecologically demanding processing of FR4 e-waste presented by Ryan (2023) [8] could be converted to more environmentally friendly solutions with a fully degradable substrate. The thorough reliability analysis of the material will be performed at higher TRL levels, where the quality and reliability issues will be evaluated on substrate, track and plated through hole via levels. The main drawback of this technology is its slightly reduced quality and reliability and poor environmental performance. The future may introduce further improvements with the chosen textiles and impregnates (e.g. a possible path would be to vary the impregnation oils and their postimpregnation handling), or to introduce inner copper layers to improve mechanical performance, however this is an expansive path for the future. 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