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Recent Advances in 3D Printed Sensors: Materials, Design, and Manufacturing

Sensors are of great importance in different aspects of research and industry. Future sensors will require high-efficient and low-cost manufacturing, as well as high-performance functionality in areas, such as mechanical sensing, biomedical, and optical applications. Recent advances in 3D printing open a new paradigm for sensors fabrication as a precision, customizable, and seamless process. Here, in this article, the state-of-the-art 3D printing methods in sensors manufacturing is reviewed and the performance of the 3D printed sensing materials and devices is summarized. Special attention is paid to emerging multimaterial printing and 4D printing technologies, which will benefit the fabrication of a new generation of structures with multifunctionalities. The content on 3D printed sensors covers piezoelectric sensors, medical, and optical sensing devices. The performance of 3D printed sensors in comparison with the sensors made by traditional manufacturing is also covered. Finally, section 4 provides the viewpoints on the future development of 3D printed sensors.

36 MATERIALS SCIENCE↗

Aerosol-Jet Printed Sensors for Environmental, Safety, and Health Monitoring: A Review

An emergent direct-write approach, aerosol-jet printing (AJP), is gaining attention for the deployment of rapid and affordable microadditively manufactured energy-efficient sensors and printed electronics. AJP enables a broad range of ink viscosities (0.001–1 Pa s) for printing diverse materials ranging from ceramics and metals to polymers and biological matter. Reproducible, high-spatial-resolution features (≈10 µm), and wide standoff distances (1–11 mm) between the nozzle and the substrate facilitate conformal printing of complex geometrical designs on nonplanar—e.g., stepped or curved—surfaces. Here this paper aims to provide a comprehensive overview of state-of-the-art AJP-based sensors (e.g., strain and temperature gauges, biosensors, photosensors, humidity and surface acoustic wave sensors, dielectric elastomer actuators, and motion, smoke, and hazardous gas detectors) and to discuss prospective applications. The drive toward cost-effective devices that are smaller, lighter, and better-performing remains a frontier challenge in the field of printed electronics. Consequently, as AJP becomes increasingly utilized in the high-volume manufacturing of miniaturized active and passive sensors, it opens a pathway for facile large-scale fabrication of devices for a wide range of consumer and industrial applications, including transportation, agriculture, infrastructure, aerospace, national defense, and healthcare.

3-dimensional↗

Robustness and printed sensor qualification

A limiting factor of additive manufactured (AM) sensors for in-pile applications is the development of appropriate interconnection and packaging strategies that can maintain reliable performance in extreme environments. Failure mechanisms in these harsh conditions could include, but not limited to, materials interaction (i.e., intermetallic formation) and coefficient of thermal expansion (CTE) mismatch between the individual components of the sensors. To mitigate premature failure and enable the successful sustained operation of AM sensors, non-destructive qualification tests are used as an intermediate process control step used for verifying robustness and reliability of the sensor before they are deployed. A materials system of interest is the use of barium strontium titanium oxide (BST) films on stainless steel 316L (SS316L) substrate. Due to BST’s high dielectric constant and tunable dielectric properties, there is an interest for its application as an insulation/encapsulation layer for capacitive strain gauges when printed on structural materials. Previous work on the BST/SS316L material system, however, showed that the BST cracks when exposed to temperatures up to 600 °C due to CTE mismatch between the printed BST film and the metallic substrate. When comparing different fabrication techniques, less surface cracking was observed in the samples that deposited thinner (i.e., 2-20 μm) than samples that were thicker (i.e., 135 µm – 300 µm). The objective of this report is to establish a qualification process that will determine and address any challenges (i.e., mechanical failure of thick prints) of the AM sensor prior to its application in experimental tests. To demonstrate the qualification process in this report, laser spallation and uniaxial tensile tests using dynamic and quasi-static loading, respectively, will be discussed.

36 - MATERIALS SCIENCE↗

Enabling In-Core Strain Measurement: Printed Sensors for Advanced Reactors

Advances in nuclear energy systems require an improved understanding of fuels, cladding, and structural materials; however, the extreme environmental conditions at irradiation test facilities often limit mechanical property evaluation to post-irradiation examination. In-situ monitoring techniques can accelerate materials qualification by providing direct insight into real-time material behavior during irradiation testing. Additively manufactured (AM) strain gauges offer a compact, material-compatible alternative to commercial sensors, particularly where space constraints, attachment limitations, or material compatibility requirements complicate conventional sensor use. This poster presents an overview of the development and testing of AM strain gauges in nuclear-relevant environments, demonstrating their potential to enhance structural health monitoring capabilities during irradiation experiments.

36 - MATERIALS SCIENCE↗

Laser-based Adhesion Strength Measurements for Advanced Manufactured Sensor Adhesion Characterization

As part of the advanced manufacturing (AM) focus of the Nuclear Energy Enabling Technologies (NEET) Advanced Sensors and Instrumentation (ASI) Program, new in-house capabilities to fabricate and test novel active and passive in-pile sensors are being developed at the Idaho National Laboratory (INL). These advanced-manufactured sensors, such as peak temperature monitors and strain gauges, must be miniaturized and be able to provide real-time feedback, all while withstanding the coupled extremes of temperature and radiation typically observed in the environment of a nuclear test reactor. Fabricating durable and robust in-pile sensors with high fidelity requires a fundamental understanding of the optimal process parameters required in the AM technique, as well as the effect of deviations from optimal process parameters on the sensor-substrate adhesion and the ultimate robustness of the sensor. This report presents the use of a laser-based, non-contact approach for characterizing the adhesion of sensors manufactured using aerosol jet printing (AJP) that comprise of silver nanoparticle inks deposited and sintered on austenitic stainless steel (SS) 316L substrates. The effect of substrate surface roughness, surface energy, ink sintering time and sintering temperature on the printed sensor topography and the sensor-substrate adhesion has been systematically investigated. The sensor-substrate interfacial adhesion strength was determined from the critical laser pulse energy required to ablate/ detach the printed sensor from the substrate. Measurements of the sensor topography using optical profilometry revealed that post-deposition sintering at 400°C for 60 minutes resulted in a reduced sensor thickness, while plasma treating the substrate prior to printing yielded sensors with uniform thickness profiles transverse to the print direction. Sintering temperature and time were found to be the dominant parameters that affected sensor-substrate adhesion, followed by substrate surface roughness. The laser-based and locally-destructive approach for adhesion strength measurements shows promise in overcoming the challenges and limitations of current standardized peel tests and can be developed into a post-fabrication process control protocol for evaluating the durability of AM printed sensors in a high throughput fashion. Future studies will investigate the use of laser-induced spallation techniques as well as non-destructive laser ultrasonic methods for sensor-substrate adhesion characterization on sensors manufactured using AJP and other AM techniques such as plasma jet printing (PJP).

42 ENGINEERING↗

3D Printed Chromophoric Sensors

Eight chromophoric indicators are incorporated into Sylgard 184 to develop sensors that are fabricated either by traditional methods such as casting or by more advanced manufacturing techniques such as 3D printing. The sensors exhibit specific color changes when exposed to acidic species, basic species, or elevated temperatures. Additionally, material properties are investigated to assess the chemical structure, Shore A Hardness, and thermal stability. Comparisons between the casted and 3D printed sensors show that the sensing devices fabricated with the advanced manufacturing technique are more efficient because the color changes are more easily detected.

3d printing↗

Fully‐Printed Ion Sensor Arrays for Measuring Agricultural Nitrogen and Potassium Concentrations Using Nernstian and AI Models

Abstract The chemical composition of growing media is a key factor for plant growth, impacting agricultural yield and sustainability. However, there is a lack of affordable chemical sensors for ubiquitous nutrient ion monitoring in agricultural applications. This work investigates using fully printed ion‐sensor arrays to measure the concentrations of nitrate, ammonium, and potassium in mixed‐electrolyte media. Ion sensor arrays composed of nitrate, ammonium, and potassium ion‐selective electrodes and a printed silver‐silver chloride (Ag/AgCl) reference electrode are fabricated and characterized in aqueous solutions in a range of concentrations that encompass what is typical for agricultural growing media (0.01 m m –1 m ). The sensors are also tested in mixed‐electrolyte solutions of NaNO 3 , NH 4 Cl, and KCl of varying concentrations, and the recorded potentials are input into Nernstian and artificial neural network models to compare the prediction accuracy of the models against ground truth. The artificial neural network models demonstrated higher accuracy over the Nernstian model, and the model using only ion‐sensor inputs is 7.5% more accurate than the Nernstian model under the same conditions. By enabling more precise and efficient fertilizer application, these sensor arrays coupled to computational models can help increase crop yields, optimize resource use, and reduce environmental impact.

Goodrich, Payton [University of California Berkele↗

Direct Mercury Detection in Landfill Leachate Using a Novel AuNP-Biopolymer Carbon Screen-Printed Electrode Sensor

A novel Au nanoparticle (AuNP)-biopolymer coated carbon screen-printed electrode (SPE) sensor was developed through the co-electrodeposition of Au and chitosan for mercury (Hg) ion detection. This new sensor showed successful Hg2+ detection in landfill leachate using square wave anodic stripping voltammetry (SWASV) with an optimized condition: a deposition potential of −0.6 V, deposition time of 200 s, amplitude of 25 mV, frequency of 60 Hz, and square wave step voltage of 4 mV. A noticeable peak was observed at +0.58 V associated with the stripping current of the Hg ion. The sensor exhibited a good sensitivity of ~0.09 μA/μg (~0.02 μA/nM) and a linear response over the concentration range of 10 to 100 ppb (50–500 nM). The limit of detection (LOD) was 1.69 ppb, which is significantly lower than the safety limit defined by the United States Environmental Protection Agency (USEPA). The sensor had an excellent selective response to Hg2+ in landfill leachate against other interfering cations (e.g., Zn2+, Pb2+, Cd2+, and Cu2+). Fifteen successive measurements with a stable peak current and a lower relative standard deviation (RSD = 5.1%) were recorded continuously using the AuNP-biopolymer-coated carbon SPE sensor, which showed excellent stability, sensitivity and reproducibility and consistent performance in detecting the Hg2+ ion. It also exhibited a good reliability and performance in measuring heavy metals in landfill leachate.

Hwang, Jae-Hoon (ORCID:0000000220100864)↗

Development of Quality Control Methods for Robust and Reliable Sensor Design

The successful adoption of additive manufacturing for the rapid prototyping of printed sensors requires the establishment of quantifiable metrics that can interrogate device performance. One measure of performance is the adhesion strength between the substrate and sensor interface, which is critical since the strength of this interface can dictate the accuracy and reliability of the printed sensor. In this work, a non-contact laser-induced spallation technique was used to quantify the adhesion of silver prints on an aluminum alloy substrate. The laser-based method was compared to a standardized pull-off adhesion test, which provided baseline measurements of adhesion strength. The sintering conditions were shown to play an important role in the film-substrate adhesion strength, as well as the cohesion and ductility of the film itself. The methods and results described in this work supports the establishment of process control steps that are necessary for verifying the reliability of printed devices prior to its deployment in critical experiments.

36 MATERIALS SCIENCE↗

The Influence of Microstructure on TCR for Inkjet-Printed Resistive Temperature Detectors Fabricated Using AgNO 3 /Ethylene-Glycol-Based Inks

This study investigated the influence of microstructure on the performance of Ag inkjet-printed, resistive temperature detectors (RTDs) fabricated using particle-free inks based on a silver nitrate (AgNO 3 ) precursor and ethylene glycol as the ink solvent. Specifically, the temperature coefficient of resistance (TCR) and sensitivity for sensors printed using inks that use monoethylene glycol (mono-EG), diethylene glycol (di-EG), and triethylene glycol (tri-EG) and subjected to a low-pressure argon (Ar) plasma after printing were investigated. Scanning electron microscopy (SEM) confirmed previous findings that microstructure is strongly influenced by the ink solvent, with mono-EG inks producing dense structures, while di- and tri-EG inks produce porous structures, with tri-EG inks yielding the most porous structures. RTD testing revealed that sensors printed using mono-EG ink exhibited the highest TCR (1.7 × 10 -3 /°C), followed by di-EG ink (8.2 × 10 -4 /°C) and tri-EG ink (7.2 × 10 -4 /°C). These findings indicate that porosity exhibits a strong negative influence on TCR. Sensitivity was not strongly influenced by microstructure but rather by the resistance of RTD. The highest sensitivity (0.84 Ω/°C) was observed for an RTD printed using mono-EG ink but not under plasma exposure conditions that yield the highest TCR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Towards P3HT Inkjet Printability of Sensors

Here we propose a method to inkjet print sensors using P3HT and present the data that demonstrates the printability potential of this material. Poly(3-Hexylthiophene) commonly known as P3HT is a semiconductor polymer that is usually used as a hole transporting material in the fabrication of transistors, and perovskite solar cells. There is a desire to transpose this technology to inkjet printing to ease the testing and researching of semiconductor polymers. However, there has been not success in the inkjet printability of P3HT due to the lack of key information such as viscosity and surface tension and the additional issues of using a strong solvent to dilute P3HT. In this work we propose a method to inkjet print P3HT sensors using a commercially available inkjet printer. This method is reinforced with the measurements obtained from a viscometer and surface tensiometer.

Marquez, Jesus↗

Additive manufacturing and applications of nanomaterial-based sensors

Nanoscale materials possess distinct physical and chemical attributes including size-dependent properties, quantum confinement, high surface-to-volume ratio, and superior catalytic activity. These unique qualities enable sensors with high sensitivity, robustness, and fast time response. As the emergence of the Internet of Things (IoT) demands increased production of sensors, it also provides an impetus for concentrated nanomaterial-based sensor research. Meanwhile, additive manufacturing (AM) of nanomaterial-based sensors is critical to bridge the gap between one-off, lab-scale fabrication and cost-effective, industrial-scale production with high reproducibility. By applying the design flexibility and cost savings of AM techniques, a new generation of nanomaterial-based sensing platforms can be integrated with IoT devices in the consumer space. Furthermore, emergent research in human-machine interfaces, food safety, and point-of-care diagnostics will be expedited by the development of sensors that can be printed with irregular form factors. In this Review, the relative strengths and weaknesses of printed sensor systems based on zero-, one-, and two-dimensional nanomaterials are discussed. In addition, sensors enabled by printable soft nanomaterials, heterostructures, and nanocomposites are surveyed due to their synergistic advantages for wearable healthcare monitoring and soft robotics. Lastly, a roadmap for the next decade of research on this topic is provided.

36 MATERIALS SCIENCE↗

Aerosol jet printed 3 omega sensors for thermal conductivity measurement

The 3 omega (3ω) method is a trusted technique for measuring thermal conductivity—a fundamental material property of critical importance in a broad range of applications. However, traditional 3ω sensor processing requires some form of physical vapor deposition, such as metal evaporation or sputtering. These 3ω sensor deposition techniques limit the materials and sample sizes applicable to the 3ω method. This work demonstrates an aerosol jet printing method to directly print silver 3ω sensors that yield accurate temperature-dependent measurement up to 300 °C on materials with thermal conductivity ranging from 1 to 150 W/m K. The interrelationship between printed sensor geometry, sensor thermal stability, and applicability to the 3ω method is examined. Thermal conductivity measurement with 3ω sensors conventionally sintered at 300 °C agrees to independent laser flash measurement within 4% from room temperature to 150 °C. An unconventional rapid high-temperature sintering method is shown to produce sensors that agree within 3% of the laser flash measurements from room temperature to 300 °C. The rapid sintering profiles also reduced the sensor–substrate thermal boundary resistance of the printed sensors by as much as 88%. The direct printing of 3ω sensors creates opportunities for measurement of thermal transport properties in applications previously inapplicable to the 3ω method.

47 OTHER INSTRUMENTATION↗

Performance of Embedded Sensors in 3D Printed SiC

This report summarizes recent advances in embedding sensors in 3D printed silicon carbide (SiC) ceramic components under the Transformational Challenge Reactor (TCR) program. The additive manufacturing technologies developed under this program will enable fabrication of complex structures with embedded fuels and sensors. The sensors will be capable of characterizing fuel performance using spatially distributed measurements at the most strategic locations that would be otherwise inaccessible using conventional manufacturing techniques. While previous programmatic updates describe initial concepts for embedding sensors, materials selection, and initial characterization of the embedded sensors, the technology requires further demonstration, and quality-significant procedures must be established before the embedding technology is ready for adoption by industry. To this end, this report describes the most effective techniques that have been used to embed functional sensors in 3D printed components using a combination of binder-jet additive manufacturing and chemical vapor infiltration (CVI). A detailed procedure describes each step in the process and is available upon request. Molybdenum (Mo)-sheathed thermocouples have been successfully embedded in complex SiC components, and temperatures were monitored in situ during the embedding process. Post-embedding measurements showed no significant hysteresis, and characterization of the interface revealed qualitatively strong bonding around the entire perimeter of the sensor sheath. Distributed fiber-optic temperature sensors were able to briefly measure temperature profiles during CVI, but they ultimately failed prior to completion of the CVI run. The failure appears to be related to the fiber coating at temperatures close to 1,000°C. Future work will focus on irradiation testing of embedded thermocouples and other sheathed electrical sensors, as well as the identification of fiber-optic sensor coatings that can survive CVI.

42 ENGINEERING↗

Printed Potentiometric Nitrate Sensors for Use in Soil

Plant-available nitrogen, often in the form of nitrate, is an essential nutrient for plant growth. However, excessive nitrate in the environment and watershed has harmful impacts on natural ecosystems and consequently human health. A distributed network of nitrate sensors could help to quantify and monitor nitrogen in agriculture and the environment. Here, we have developed fully printed potentiometric nitrate sensors and characterized their sensitivity and selectivity to nitrate. Each sensor comprises an ion-selective electrode and a reference electrode that are functionalized with polymeric membranes. The sensitivity of the printed ion-selective electrodes was characterized by measuring their potential with respect to a commercial silver/silver chloride reference electrode in varying concentrations of nitrate solutions. The sensitivity of the printed reference electrodes to nitrate was minimized with a membrane containing polyvinyl butyral (PVB), sodium chloride, and sodium nitrate. Selectivity studies with sulphate, chloride, phosphate, nitrite, ammonium, calcium, potassium, and magnesium showed that high concentrations of calcium can influence sensor behavior. The printed ion-selective and reference electrodes were combined to form a fully printed sensor with sensitivity of −48.0 ± 3.3 mV/dec between 0.62 and 6200 ppm nitrate in solution and −47 ± 4.1 mV/dec in peat soil.

Baumbauer, Carol L. (ORCID:0000000246747551)↗