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Method Article
Here, we present a protocol for the design, manufacture, and use of a simple, versatile 3D-printed and controlled atmospheric chamber for the optical and electrical characterization of air-sensitive organic optoelectronic devices.
In this manuscript, we outline the manufacture of a small, portable, easy-to-use atmospheric chamber for organic and perovskite optoelectronic devices, using 3D-printing. As these types of devices are sensitive to moisture and oxygen, such a chamber can aid researchers in characterizing the electronic and stability properties. The chamber is intended to be used as a temporary, reusable, and stable environment with controlled properties (including humidity, gas introduction, and temperature). It can be used to protect air-sensitive materials or to expose them to contaminants in a controlled way for degradation studies. To characterize the properties of the chamber, we outline a simple procedure to determine the water vapor transmission rate (WVTR) using relative humidity as measured by a standard humidity sensor. This standard operating procedure, using a 50% infill density of polylactic acid (PLA), results in a chamber that can be used for weeks without any significant loss of device properties. The versatility and ease of use of the chamber allows it to be adapted to any characterization condition that requires a compact-controlled atmosphere.
Organic and perovskite optoelectronic devices, solar cells, and light-emitting diodes based on π-conjugated semiconducting organic molecules and organometal halides are a rapidly growing field of research. Organic light-emitting diodes (OLEDs) are already a major technological element in lighting and displays1, and organic photovoltaics have begun to achieve efficiencies that make them competitive with amorphous silicon2. The recent rapid advancement of perovskite-based devices for light absorbing and light-emitting applications3,4,5 suggests that low-cost, easily processed devices are likely to soon find widespread deployment. However, all of these technologies suffer from a sensitivity to atmospheric contaminants, particularly moisture and oxygen, which limits their effective lifetimes6,7,8,9.
For researchers studying such systems, it can be useful to have an adaptable, easy-to-use, portable, and reusable chamber to protect such sensitive materials or to expose them to contaminants in a controlled manner10,11. Though it is possible to use a glovebox for the characterization of air-sensitive devices, these large, expensive, and fixed-location, inert environments may be incompatible with the wide range of characterization that might be required. To provide a portable alternative, Reese et al.10 proposed a small metal chamber based on a standard vacuum flange suitable for the electrical and optical characterization of organic devices. We have adapted this design, making it cheaper and more versatile by using 3D-printing to produce the chamber components. The use of 3D-printing, rather than machining, allows for rapid, cost-effective adjustments to changing sample or environmental requirements while maintaining the utility of the basic design. In this contribution, we outline the procedure to make such a chamber, and use it to extract the current-voltage characteristics of an organic diode device.
A good encapsulation of organic and perovskite devices should have WVTRs of 10-3 - 10-6 g/m2/day for long-term device stability12,13, to ensure little water ingress into the organic device even in very harsh conditions. As this chamber is designed to be a controlled environment for testing purposes rather than a long-term storage or encapsulation method, the requirements for an effective chamber are not as strict. The chamber should be able to maintain the device properties within a reasonable timeframe to perform characterization experiments. The standard operating procedure of using PLA results in a chamber which can be used for several days or even weeks with an incorporated gas flow, without a significant loss of the device properties.
Changing the materials, or even the shape and size of the chamber body can drastically affect the penetration of contaminants from the air into the chamber. Therefore, the ingress of moisture and oxygen needs to be carefully monitored for each design to determine the efficacy of the chamber. We, additionally to the fabrication of the chamber, outline a simple procedure for determining the WVTR of the chamber, using a commercially available humidity sensor, to establish a timeframe for the use of the chamber for experimentation.
Such a simple, yet versatile chamber allows for multiple types of experiments to be performed. They can act as inert atmosphere environments outside the glovebox, suitable for electrical and optical characterizations through the electrical feedthrough ports and window. Their portability allows them to be used with standard electrical characterization equipment outside the lab where they were manufactured, which is useful in round robin testing for reliability14 or to obtain certified measurements of the device performance15. These chambers are also particularly useful for studying the effects of the introduction of contaminants for controlled degradation tests, with simple modifications. The use of 3D printing allows a significant, rapid adaptability to changing device layouts, sizes, or testing requirements.
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1. The 3D Print Chamber Parts
Note: All printer preparation, “slicer” software settings, and print parameters were specific to the printer indicated in the Table of Materials. There is a wide array of 3D printers, each with their own set of preparation steps and optimal parameters. There is also a wide array of colors possible for the polymer filament used for the printed parts. It is not required to use the same plastic for each part.
Figure 1: A configuration table with an exploded view of the test chamber. (a) This table shows the .stl files for various chamber configurations. The rows show 3D-rendered schematics of the variations on each chamber part to be printed. The columns show the necessary parts to complete a single chamber. Note that a chamber will have either a bottom chamber or a bottom chamber with gas ports, not both. (b) This panel shows an exploded CAD view of a printed chamber for a 4-pixel IV test configuration. Note that the O-ring, the organic device, and the KF50-centering gasket are not 3D printed. Please click here to view a larger version of this figure.
Figure 2: 3D printer settings. This is a screenshot of the required machine settings in the slicing software to produce the 3D-printed parts for the chambers. Please click here to view a larger version of this figure.
2. The Top Chamber Assembly
Figure 3: The assembling of the top chamber. (a) This panel shows a disassembled 4-pixel top chamber. (b) This panel shows the application of threaded inserts in the top chamber using a soldering iron. (c) This panel shows partially assembled top chamber components showing the alignment of the retaining ring to the top chamber (note that the O-ring and the screws are not shown for clarity). Different colors of PLA plastic were used for the printing of various parts; these have no effect on the performance of the chamber. Please click here to view a larger version of this figure.
Figure 4: Possible device pixel patterns for a pin layout. These panels show the layout of the organic solar cell or light-emitting diode device used for designating the contact pin positions for (a) a 4-pixel and (b) a 6-pixel IV test chamber configuration. Each pixel is numbered with a reference to the orientation marks (green stars) for their correct placement in the chamber. Black and red circles represent the cathode and anode contacts (i.e., pin positions), respectively. Note that for the 6-pixel configuration, the top two pixels are masked by the opening in the top chamber and not numbered as only four pixels can be tested under illumination or emission conditions. (c) This panel shows the orientation of a 6-pixel device relative to the 6-pixel bottom chamber with its pin positions indicated. Please click here to view a larger version of this figure.
3. The Bottom Chamber Assembly
Note: Only follow step 3.1 if a configuration with a bottom chamber with gas flow ports is needed.
Figure 5: An assembled chamber with gas ports. This panel shows a fully assembled chamber including a bottom chamber with gas ports. The push-to-connect gas ports embedded in the available holes in the chamber are attached to tubing with gas flow control valves to control the introduction of gas. Note that the contact pins are omitted for clarity. Please click here to view a larger version of this figure.
Figure 6: A complete, assembled bottom chamber. (a) This panel shows an assembled bottom chamber for a 4-pixel IV test configuration with the contact pins seated using low-pressure epoxy suitable for vacuum applications. The brown O-ring (KF50)-centering ring gasket is used to ensure a tight fitting with the top chamber. (b) This panel shows a solder cup and pogo pin after soldering. (c) This panel shows a close-up of set epoxy, showing the correct seating of the contact pin in the bottom chamber holes. Please click here to view a larger version of this figure.
4. The Final Assembly
Note: This assembly is to be done within a glovebox environment after both the assembled top and the bottom chamber have been inside the glovebox for ≥ 24 h.
Figure 7: An assembled, complete test chamber. (a) This panel shows a fully assembled 4-pixel IV test chamber with a KF50 cast clamp ensuring a tight fit between the bottom and top chamber. The inset shows another angle of the KF50 clamp closed in the maximum tightness position. (b) This panel shows an assembly of the 4-pixel top chamber with the retaining ring (note that the O-ring is already mounted in the top chamber). Other chamber configurations are assembled in the same way. Please click here to view a larger version of this figure.
5. Conduct IV Measurements of the Individual Pixels on the Device
Note: This section details the procedure used to generate the data shown in the Representative Results. The source-measurement unit (SMU) and the Zero Insertion Force (ZIF) test board used are listed in the Table of Materials. However, any method of chamber connection to an SMU to collect current-voltage data can be used. All IV measurement steps were conducted on a Windows machine. “Pixel” refers to a single diode on the organic device.
Figure 8: The IV measure in Python. This is a screen shot of the BasicIV.py Python script with the COM port location indicated. Please click here to view a larger version of this figure.
Figure 9: The IV measurement set-up. (a) This panel shows a fully assembled chamber connected to the zero-insertion force (ZIF) test board and source measurement unit (SMU) for an IV measurement testing. (b) This panel shows the range switch "2" set in the ON position to correctly connect the device to the SMU for the measurement. Please click here to view a larger version of this figure.
6. Assemble the Chamber for WVTR Testing
Figure 10: The humidity testing setup. (a) This panel shows a completely assembled WVTR test chamber wired to internal and external DHT22 humidity sensors using a breadboard jumper to a microcontroller. (b) This panel shows the DHT22 humidity sensor inside the WVTR test bottom chamber. Note that the wires are fed through the bottom chamber and are held in place with low-pressure epoxy. (c) This panel shows a schematic of the internal and external humidity sensor DHT22 and a microcontroller board wiring diagram using a single breadboard (for convenience). The sensor is connected to the microcontroller pins "5 V" (red) and "GND" (green) to provide power to the sensor. The data output from the sensor (yellow) connects to the pins in "DIGITAL" [2 for the internal (INT) sensor and 4 for the external (EXT) sensor] with a 10 kΩ resistor. The inset shows a DTH22 sensor with the correct pin wiring: 5V (red), ground (green), and data (yellow). Please click here to view a larger version of this figure.
7. Conduct a Humidity Measurement to Determine the WVTR
Figure 11: A water vapor transmission rate screenshot. These panels show (a) a screen shot of the Run_WVTR_Test.py Python script with (b) the COM port location indicated. Please click here to view a larger version of this figure.
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Current-voltage Measurements:
This chamber is designed to allow for the testing of an air-sensitive diode device, such as an organic or perovskite solar cell or a light-emitting diode. It can act as a reusable, temporary encapsulation or as a method of introducing contaminants to perform controlled degradation testing. The current density-voltage (JV) curves shown here were measured using a ZIF test board attach...
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The critical steps in recreating this experiment include the printing of the chambers to avoid cracks, gaps, or poor in-fill characteristics which can decrease the WVTR, sealing the chamber to prevent any ingress of moisture and oxygen by tightening the KF50 clamp to achieve a full sealing between the top and bottom chambers, using a vacuum-rated low-pressure epoxy around the contact pins or any feedthroughs to prevent any leaking, and creating a seal between the sample and the top chamber using a proper O-ring placement...
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The authors have nothing to disclose.
The authors acknowledge Peter Jonosson and the Lyons New Media Centre for the 3D printing of the chambers. This research was supported by 436100-2013 RGPIN, ER15-11-123, the McMaster Dean of Engineering Excellence Undergraduate Summer Research Award, and the Undergraduate Research Opportunities Program.
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Name | Company | Catalog Number | Comments |
ORION DELTA DESKTOP 3D PRINTER RTP | SeeMeCNC | 87999 | Known in Report As: 3D Printer |
1.75 mm PLA Filament | SeeMeCNC | 50241 | Known in Report As: PLA |
Somos® WaterShed XC 11122 chamber | Somos | printed at Custom Prototypes, Toronto. | https://www.dsm.com/products/somos/en_US/products/offerings-somos-water-shed.html Known in Report As: Water resistant polymer |
CURA | CURA | https://ultimaker.com/en/products/cura-software Known in Report As: slicing software | |
Soldering iron with 600° F tip | Weller | WTCPT | |
Xtralien X100 Source Measure Unit | Ossila | E561 | Known in Report As: SMU |
ZIF Test Board for Pixelated Anode Substrates | Ossila | E221 | Known in Report As: Zero insetion force/ZIF Test Board; |
BNC Cable | |||
Generic USB A - B | |||
Generic USB A - Micro | |||
#12 O-Ring | Source unkown Known in Report As: o-ring | ||
116 Butyl O-Ring | Global Rubber Products | 116 VI70 | Bought in-store Known in Report As: o-ring |
Retaining ring | McMaster | NA | 3D printed in-house |
Bottom Chamber | McMaster | NA | 3D printed in-house |
Top Chamber | McMaster | NA | 3D printed in-house |
KF50 Cast Clamp (Aluminum) | Kurt J. Lesker | QF50-200-C | |
KF50 Centering Ring (Aluminum) | Kurt J. Lesker | QF50-200-BRB | |
Sn60/Pb40 Solder | MG Chemicals | 4895-2270 | |
#4-40 x 3/16" machine screw | Hardware store | ||
#4-40 IntThrd Brass TaperSingleVane Insert For Thermoplastic | Fastenal | 11125984 | Fastenal requires to be affiliated with company/university Known in Report As: #4-40 brass tapered threaded insert |
Varian Torr Seal Vacuum Equipment High Vacuum Epoxy | Vacuum Products Canada Inc. | Known in Report As: low-pressure epoxy | |
Smiths Interconnect/IDI Contact Probes HEADED RADIUS | Mouser Electornics | 818-S-100-D-3.5-G | Known in Report As: pogo pin |
Smiths Interconnect/IDI Contact Probes Receptacle Solder Cup | Mouser Electornics | 818-R-100-SC | Known in Report As: solder cup |
1/4" Teflon Tubing | Hardware store | ||
Teflon tape | Hardware store | ||
1/4" Tube x 1/8" Male NPT Nickel Plated Brass Push-to-Connect Connector | Fastenal | 442064 | Not the same ones used for this study, but are fuctionally equivalent Known in Report As: push-to-connect pneumatic connector |
1/8" NPT Tap and T-wrench | Hardware store | ||
1/4" Tube Push-to-Connect Manually Operated Valves | Fluidline | 7910-56-00 | Known in Report As: manually operated push-to-connect valves |
Adafruit DHT22 Humidity Sensor (small) | Digi-Key | 385 | Known in Report As: internal humidity sensor |
Adafruit DHT22 Humidity Sensor (large) | Digi-Key | Known in Report As: external humidity sensor | |
Arduino Uno | Arduino | ||
Glovebox environment | |||
10 kOhm Resistor | |||
Oscilla Xtralien Scientific Python IDE | Oscilla | https://www.ossila.com/pages/xtralien-scientific-python Known in Report As: Python IDE |
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