Yicong Zhao1, Shenghan Gao1, Jia Zhu2, Jiameng Li1, Hang Xu1, Kexin Xu1,3, Huanyu Cheng2,2, Xian Huang1. 1. Department of Biomedical Engineering, Tianjin University, 92 Weijin Road, Tianjin 300072, China. 2. Department of Engineering Science and Mechanics and Department of Engineering Science and Mechanics, Materials Research Institute, Pennsylvania State University, University Park, Pennsylvania 16802, United States. 3. State Key Laboratory of Precision Measuring Technology and Instruments, Tianjin University, Tianjin 300072, China.
Abstract
Communication with plants to understand their growth mechanisms and interaction with the surrounding environment may improve production yield in agriculture and facilitate prevention of plant diseases and negative influence of environmental stress. Typical sensing technologies in plant biology and precision agriculture largely rely on techniques with low spatial and temporal resolutions, and fail to continuously and precisely determine localized variation in leaf physiology and microenvironments. Here, techniques to develop a multifunctional stretchable leaf-mounted sensor have been developed to offer optimized adaptability to plant growth and monitor leaf physiological and environmental conditions in continuous and highly sensitive manners. The multifunctional leaf sensor contains multiple heterogeneous sensing elements made of metal, carbon nanotube matrix, and silicon, leading to temperature, hydration, light illuminance, and strain sensing capabilities on a leaf. Evaluation under a controlled environment indicates excellent precision and accuracy of the sensor compared to conventional devices. Furthermore, indoor and outdoor experiments have demonstrated the multifunctional monitoring ability of the sensor in real situations. The multifunctional stretchable sensor holds the promise to advance monitoring techniques in plant biology and precision agriculture, resulting in improved capability to record slow and subtle physiological changes in plants and plant/environment interaction.
Communication with plants to understand their growth mechanisms and interaction with the surrounding environment may improve production yield in agriculture and facilitate prevention of plant diseases and negative influence of environmental stress. Typical sensing technologies in plant biology and precision agriculture largely rely on techniques with low spatial and temporal resolutions, and fail to continuously and precisely determine localized variation in leaf physiology and microenvironments. Here, techniques to develop a multifunctional stretchable leaf-mounted sensor have been developed to offer optimized adaptability to plant growth and monitor leaf physiological and environmental conditions in continuous and highly sensitive manners. The multifunctional leaf sensor contains multiple heterogeneous sensing elements made of metal, carbon nanotube matrix, and silicon, leading to temperature, hydration, light illuminance, and strain sensing capabilities on a leaf. Evaluation under a controlled environment indicates excellent precision and accuracy of the sensor compared to conventional devices. Furthermore, indoor and outdoor experiments have demonstrated the multifunctional monitoring ability of the sensor in real situations. The multifunctional stretchable sensor holds the promise to advance monitoring techniques in plant biology and precision agriculture, resulting in improved capability to record slow and subtle physiological changes in plants and plant/environment interaction.
Plants contain more
than 82% of mass of all life forms on earth
and include 320 thousand species. They are not only the major determinants
to earth atmosphere and climates but also primary resources for food,
medicine, and energy. Better understating of growth mechanisms of
plants and their interaction with surrounding environments is constantly
haunting the botanists and biologists. Unlike the animal studies in
which external or internal stimulants can be rapidly reflected by
physiological signal changes and animal behaviors, the expression
of plants is silent, involving slow and subtle changes that demand
long-term and continuous observation. Many issues such as long-term
plant response under multiple stress conditions,[1,2] relationship
between stress response and plant growth,[3,4] and
early detection of plant diseases[5,6] remain unsolved,
requiring quantitative monitoring of both plant physiology and environment
conditions.The state-of-the-art technologies in precision agriculture
use
spectroscopy,[7−9] machine vision,[10−12] and airborne/satellite
surveys.[13−15] However, these techniques are low in spatial or temporal
resolutions or cannot provide timely response to events that influence
plant physiology. Emerging technologies use leaf sensors that are
either fixed on leaves with fixtures or placed in close proximity
to closely monitor leaf physiology and environmental parameters such
as water content,[16,17] leaf elongation rates,[18,19] chlorophyll,[20,21] stomatal conductance,[22,23] and temperature.[24,25] However, the rigid configurations
of these leaf sensors are mechanically incompatible to the soft and
fragile natures of leaves. Thus, these sensors are only for discrete
measurements. Recent developments of flexible electronics lead to
the development of several flexible devices[26−29] that can be attached on leaves
to measure microclimate changes. The sensor substrates, which are
typically made of polydimethylsiloxane (PDMS) and polyimide (PI),
have much higher modulus than leaves, whereas the sensor structures
lack of stretchable configurations, causing physical constraint to
the mechanics of leaves and incompetence to perform long-term monitoring.
Despite comprehensive parameters such as leaf elongation rate, water
content, stomatal conductance, temperature, light, and humidity are
crucial for botanic studies. A multifunctional sensor that can adapt
to leaf growth and simultaneously monitor leaf physiology and microclimate
has not yet been achieved.Here, we develop an ultrathin and
lightweight stretchable sensor
with multiple heterogeneous sensing elements that conduct strain,
impedance, temperature, and light intensity monitoring. The sensor,
which possesses skin-like mechanical properties, only applied <170
μN contact pressure to the leaves and deforms more than 120%
to adapt to the leaf growth. The sensor has been demonstrated to continuously
and simultaneously measure plant physiology and environmental conditions
for 2 days with little influence to the hosting plant after 45 days
integration. A wireless sensing platform can transmit the sensing
results to a distance larger than 100 m, demonstrating the capability
to form sensor networks to facilitate large-scale plant research and
precision agriculture. This paper offers innovative methods to quantify
subtle plant physiological and environmental changes, offering crucial
techniques that may eventually lead to better understanding about
the growth mechanisms of plants and their interaction with the surrounding
environment.
Results and Discussion
A typical
sensor (Figure a)
with a dimension of 13 000 × 8800 × 30
μm3 and a mass of 17 mg contains multiple heterogeneous
sensing elements made of metal, carbon nanotube (CNT), and silicon.
The sensor is fabricated by combining CMOS, printable electronics,
and transfer printing techniques, leading to hydration, temperature,
strain, and light illuminance sensing capabilities on leaves (Figure b). These elements
are connected with meshed structures, forming an island-bridge configuration
that can be engineered to optimize strain distribution within the
ultrathin composition materials when being stretched. In addition,
the self-similar serpentine interconnects that contain secondary hierarchy
structures offer stretchability that allows the entire device to synchronize
its growth with the hosting leaf. A perforated silicone membrane with
an ultralow modulus (∼3.0 kPa) supports and protects the sensor
while allowing light, gas, and water vapor to penetrate through.[30] This membrane employs a healthcare-grade material
with biocompatibility to enable excellent adhesion between the leaf
and the sensor. The adhesion of the sensor may be subjected to the
influence from rain and snow, causing the variation of adhesion forces.
To quantify the influence, the adhesion forces between the sensors
and leaves were characterized using a tensile tester by 180°
peel tests. Sensors supported by a commercial fabric (10 × 70
mm2) were attached on leaves and were peeled off mechanically
from the leaves at a speed of 50 mm·min–1.
Peel forces in situations without and with immersing the sensors on
leaves into water were obtained. As shown in Figure S1, the average peel forces are 0.32, 0.29, 0.28, and 0.27
N, respectively, corresponding to immersing times of 0, 10, 20, and
30 min. As the immersing time increased to 30 min, the average peel
force only decreased by 0.05 N, indicating that the sensor still maintains
good adhesion to the leaf under wet environment. The sensor measures
comprehensive information for better understanding the effect of photosynthesis,
plant nutrition, environmental stress, and transpiration on plant
growth and crop yield.[31] The entire sensor
can withstand different deformations (Figure c) and grow together with the host leaf in
a measurement period of 7 days (Figure d). In addition, the sensor only applies minimized
contact pressure (<170 μN) to leaves with almost no physical
constraint to leaf growth. Table compares performances and functions of this sensor
with other reported flexible leaf sensors. The leaf sensor in this
work offers larger deformation and multifunctions that allow comprehensive
assessment of relation between environmental conditions and plant
growth, while minimizing the interference to the hosting plants.
Figure 1
Schematics
and demonstration of a multifunctional stretchable sensor
on a leaf. (a) Schematic diagram and exploded view of a leaf sensor.
(b) Top view of the leaf sensor. (c) A sensor can adapt to the morphology
of a corn leaf and deform together with the leaf. (d) A sensor attached
on a leaf grows together with the leaf throughout 7 days.
Table 1
Comparison of Flexible Leaf Sensors
in Previous Studies
substrate
flexible/stretchable
functions
size (mm2)
thickness (μm)
refs
photo paper
flexible
temperature
>5
>100
(32)
resin
flexible
bioelectric potentials
>2
>100
(27)
PI/PET
flexible
drought stress
>1.1
∼100
(33)
PI
flexible
relative humidity
∼10
>100
(34)
PDMS
flexible/∼22%
temperature and humidity
∼3
>50
(29)
Silbione RT Gel 4717
flexible/up to 120%
temperature, light intensity, hydration, and leaf growth
∼1.1
∼30
this work
Schematics
and demonstration of a multifunctional stretchable sensor
on a leaf. (a) Schematic diagram and exploded view of a leaf sensor.
(b) Top view of the leaf sensor. (c) A sensor can adapt to the morphology
of a corn leaf and deform together with the leaf. (d) A sensor attached
on a leaf grows together with the leaf throughout 7 days.The multifunctional
sensor has been evaluated under controlled
indoor environments. All sensing elements were individually characterized
and calibrated with known parameters. The characterization of the
hydration sensing element was conducted by attaching a piece of filter
paper with known water contents onto the sensor. The filter paper
was first soaked with a saturated amount of water, followed by water
evaporation over time, resulting in changes in hydration levels in
the paper. Figure a shows varied impedance with changing hydration levels at different
frequencies. Changes of impedance are 2.85 MΩ at 10 kHz and
0.29 MΩ at 100 kHz, indicating that the impedance measured at
lower frequencies may offer better sensitivity and resolution. As
subsequent experiments were conducted using a miniaturized measurement
circuit (Figures h
and S2), which has a fixed impedance measurement
range from 200 to 600 kΩ. Therefore, to tolerate potential hydration
variation and fabrication variation of different batches of devices,
impedance was measured at a fixed frequency of 50 kHz, which offered
both a large hydration measurement range and a relatively high measurement
resolution. As shown in Figure b, more than 95% reduction in the magnitude of the impedance
has been observed when the hydration levels change from 0 to 100%
at a frequency of 50 kHz.
Figure 2
Characterization of individual components and
an experimental circuit.
(a) Impedance measured by the hydration sensing element between 10
and 100 kHz with varied water contents. (b) Impedance values at 50
kHz with varied water contents. (c) Responses of the temperature sensing
element to changing temperature from 9 to 62 °C. A strain sensing
component was evaluated by stretching both sensors uniaxially along
(d) x- and (e) y-directions. (f)
Height and surface profile of the phototransistor measured by a surface
profilometer after grinding. (g) Collector-emitter current of the
phototransistor with changing light intensity from 0 to 100 klux (scale
bars in figures b, c, d, f, and g represent 500 μm). (h) Exploded
view of the wireless sensing circuit that consists of stacked printed
circuit board (PCB) layers. (i) A sensing circuit is connected to
a leaf sensor with (j) screen-printed flexible cable. (k) Signal power
transmitted by a Zigbee module received in different distances.
Characterization of individual components and
an experimental circuit.
(a) Impedance measured by the hydration sensing element between 10
and 100 kHz with varied water contents. (b) Impedance values at 50
kHz with varied water contents. (c) Responses of the temperature sensing
element to changing temperature from 9 to 62 °C. A strain sensing
component was evaluated by stretching both sensors uniaxially along
(d) x- and (e) y-directions. (f)
Height and surface profile of the phototransistor measured by a surface
profilometer after grinding. (g) Collector-emitter current of the
phototransistor with changing light intensity from 0 to 100 klux (scale
bars in figures b, c, d, f, and g represent 500 μm). (h) Exploded
view of the wireless sensing circuit that consists of stacked printed
circuit board (PCB) layers. (i) A sensing circuit is connected to
a leaf sensor with (j) screen-printed flexible cable. (k) Signal power
transmitted by a Zigbee module received in different distances.A temperature sensing element
that contains a meander structure
has been calibrated using a Peltier heater that offers temperature
ranging from 9 to 62 °C. As shown in Figure c, resistance increases by 4.3% as the temperature
rises from 22 to 62 °C and decreases by 1.5% as the temperature
drops from 22 to 9 °C. The result indicates that resistance of
the temperature sensing element changes linearly with the temperature.
The temperature coefficient of resistance α is determined to
be ∼1100 ppm/°C, according to the linear relationship
between resistance and temperature R = R0[1 + α(T – T0)], where R0 is the resistance
at reference temperature of T0 and R is the resistance at temperature of T. The strain sensing element, which contains two perpendicular CNTs
strain gauges (denoted as S1 and S2 in insets of Figure d,e), has been evaluated by
stretching the sensing element uniaxially along x- and y-direction. The results of uniaxial strain
sensing element exhibit strong orientation-dependent. As shown in Figure d, S1 exhibits 15.6%
variation in resistance under 130% stretching along x-direction, whereas S2 varies only 4.2%. By contrast, a strain of
60% along y-direction leads to an increase in resistance
of S2 by 55% and only 8.6% variation in S1 (Figure e). The varied gauge factors along different
directions are caused by different clamping positions in x- and y-direction during the experiments, resulting
in different sensor responses to the same levels of overall strain.A silicon-based phototransistor has been evaluated in response
to various environmental light intensity. The phototransistor was
mechanically polished from a thickness of 200 μm to only 20
μm, resulting in a thin-film flexible phototransistor (Figure f). Sensor’s
response to varied light intensity has been conducted before and
after the thinning process, as indicated in Figure g. The collector-emitter current appears
a logarithmic increase with increased light intensity from 0 to 60
klux when the collector voltage is fixed at 3.3 V. Comparing with
the phototransistor before polishing, the thinning process leads to
at least 41.0% reduction in the photoelectric current because of reduced
numbers of charge carriers when the same amount of photonic energy
is received. However, as long as the signal–noise ratio is
allowed, the reduced photocurrent can be compensated by increasing
the gain in the external sensing circuit. The measurement of illuminance
is susceptible to various influencing factors such as wind, shadowing,
and bending. Therefore, the time resolution of the sensor should be
optimized to precisely record the influence from the above-mentioned
factors, allowing better identification between the measurement abnormity
and actual environmental light conditions. In addition, the sensor
may need to be attached onto a proper leaf of a plant to reflect the
general light exposure of the entire plant. To demonstrate applications
of the multifunctional device for real-time monitoring, a miniaturized
multifunctional sensing circuit equipped with wireless transfer capability
was developed (Figure h). The circuit, which is 3 × 3 × 2.5 cm3 in
its dimension, consists of four stacked PCBs and uses the Zigbee protocol
to enable long-range data transmission. The wireless sensing circuit
connected with a leaf sensor through a flexible cable (Figure i), which contains nine screen-printed
silver conductors on a polyethylene terephthalate (PET) substrate
(Figure j). Signal
power received in varied distances to the sensing circuit were measured.
The result demonstrates that the received power changes from ∼−15
to −65 dBm (Figure k) when the distance changes from 1 to 200 m, indicating that
the system can work in a network with a node-to-node distance at least
at 200 m, which are ideal in an open-field environment in precision
agriculture applications. The communication distance can be further
enhanced by adding radio-frequency power amplifiers on either the
transmitting or receiving side.Mechanical deformation of the
stretchable sensor under stretching
was investigated by the FEA. Simulations of four sensing elements
were conducted separately to reduce model sizes. As copper possesses
lower fracture strain (∼6%)[36] comparing to PI,[37] the stretchability of the sensor is mainly determined by strain
distributions in the copper layer. As shown in Figure a, the stretching causes both out-of-plane
and in-plane bending of serpentine interconnects to release the strain.
The maximum strain of the sensor (∼6.2%) is mainly located
on arcs of the serpentine interconnects with the largest radius of
curvature under 150% stretching in x-direction; the
results are consistent with previous studies[38] as well as device images obtained by applying strains through a
mechanical stretcher. A maximum strain of ∼6.1% in response
to 60% stretching in y-direction can also be observed
on serpentine structures with the largest radius of curvature (Figure b). The maximum stretchability
along the y-direction is, thus, determined to be
60%, which can be improved by introducing higher orders of self-similar
serpentine interconnects.
Figure 3
Mechanical study of the multifunctional stretchable
sensor. Finite
element analysis (FEA) and experimental images of serpentine interconnections
under mechanical stretching (a) along y-direction
with a strain of 150% and (b) along x-direction with
a strain of 60%.
Mechanical study of the multifunctional stretchable
sensor. Finite
element analysis (FEA) and experimental images of serpentine interconnections
under mechanical stretching (a) along y-direction
with a strain of 150% and (b) along x-direction with
a strain of 60%.To demonstrate multifunctional
monitoring ability of the stretchable
sensor, experiments that measured leaf physiology continuously were
first conducted in an indoor environment on a Scindapsus
aureus (S. aureus)
leaf in 2 days (Figure a–d). During the experiment, external conditions involving
cooling, wind blowing, fog generation, water spraying, and light switching
were deliberately introduced to evaluate sensor response. As shown
in the temperature measurement result (Figure a), the sensor can timely respond to four
different external conditions that induce rapid temperature changes
as large as 4.9 °C in the local environment. In addition, the
sensor is also able to monitor temperature changes that caused by
natural conditions, resulting in a slow change in room temperature
of 5.4 °C in a day. By considering the signal-to-noise ratio
and resolution of the sensing circuit, the temperature sensing element
can offer a temperature sensing resolution of 0.2 °C. During
the environmental light illuminance measurement, the environmental
lighting was controlled by in-door lighting and external sunlight.
It can be observed that the sensor has very sensitive responses to
both light sources (Figure b). Its response closely follow the variation of sunlight
during the day and instantly adapt to the change in in-door lighting
after switching off the light. External factors such as wind blowing
can only cause less than 3.0% signal variation, which is negligible
when considering the overall signal variation (Δ = 1678 lux)
determined by environmental lighting. The hydration sensing element
has also demonstrated stable response to slow hydration changes on
the leaf as well as rapid environmental humidity changes caused by
fog generation and water spraying (Figure c). In comparison, the sensor exhibits a
negligible signal variation of less than 0.6% in response to the wind
blowing event, which is considered barely alternate both environmental
humidity and leaf hydration. A reference measurement that eliminated
environmental influence using a leaf cutoff from the plant indicates
that the impedance maintains increasing over a period of 3 days. The
increase in impedance was mainly caused by the dehydration process
of the leaf (Figure S3). The result of
strain sensing indicates that the leaf grew steadily during the test
(Figure d). It is
noticeable that the growth of the leaf is mainly in the width (y-direction), causing large deformation (15.5%) of the sensor
in the y-direction (Figure e) as compared with 2.4% strain in the x-direction. Again, the strain sensing element exhibits
excellent robustness to withstand external wind blowing, as the resistance
variation due to wind blowing is only 0.9%. It has been observed that
the resistance of the sensor along the y-direction underwent a rapid
increase on the second day between 23:00 PM and 05:00 AM, indicating
a potential rapid leaf growth event during the night. The strain sensing
results, as well as other experiments, conducted in-door demonstrate
the multiparameter sensing capability of the sensor in response to
various events. These parameters can be combined to determine the
growth conditions of leaves and reveal factors that can influence
leaf growth.
Figure 4
Characterization of multifunctional leaf sensors indoor
and outdoor.
Results of (a) ambient temperature, (b) light intensity, (c) hydration,
and (d) strains measured by a leaf sensor on a Scindapsus
aureus leaf obtained in a period of 2 days. (e) Images
of the strain sensor before and after the measurement are also shown.
Synchronized measured results of (f) ambient temperature, (g) light
intensity, (h) hydration, and (i) strain measured by a leaf sensor
on a corn leaf. (j) Images of a multifunctional leaf sensor attached
on a corn leaf and the measurement circuit during the outdoor measurement.
Characterization of multifunctional leaf sensors indoor
and outdoor.
Results of (a) ambient temperature, (b) light intensity, (c) hydration,
and (d) strains measured by a leaf sensor on a Scindapsus
aureus leaf obtained in a period of 2 days. (e) Images
of the strain sensor before and after the measurement are also shown.
Synchronized measured results of (f) ambient temperature, (g) light
intensity, (h) hydration, and (i) strain measured by a leaf sensor
on a corn leaf. (j) Images of a multifunctional leaf sensor attached
on a corn leaf and the measurement circuit during the outdoor measurement.A similar leaf sensor was then
attached on a leaf of a corn for
preliminary outdoor experiments (Figure f–j). All data are synchronized to
reveal potential influencing factors to the growth of the corn. The
temperature variation measured by the sensor can closely follow the
temperature measured by a thermal camera (Figure f). The decreased environmental temperature
of 2.3 °C during the measurement period has been recorded. Correspondingly,
the environmental light illuminance also follows the patterns similar
to the temperature measurement. The complete sunset appears at around
8 PM indicated by changes in the environmental light illuminance changes
from 18.2 to 1.1 lux (Figure g), which is also confirmed by referring to the local meteorological
data. Because of the reduced sun exposure and temperature decrease,
the transpiration effect within the leaf is believed to be reduced.
As a result, the hydration within the leaf is increased as the impedance
reduces from 228.3 to 200.2 kΩ (Figure h). A time delay can be observed between
light and temperature decrease and hydration increase. This may
be due to the biological response of corn and may be interesting to
be further examined in future research. Despite changes in temperature,
light illuminance, and hydration, the signals from the strain sensing
element are very steady with noise less than 3% (Figure i). Because of the relative
short measurement period, no significant changes in strains along
both the x- and y-direction have
been observed. The results from the outdoor experiments indicate that
the leaf sensor can work in outdoor environments and multichannel
sensing results can serve as important parameters for analyzing environmental
influence and leaf biology. Outdoor experiments over an extended measurement
period will be conducted in future research to reveal environmental
and intrinsic factors that will influence the plant growth.The biological effect of leaf sensors to leaves has been studied
using the changes in the morphology of the leaf stomas, which are
vital organs to regulate transpiration and gas exchange between leaves
and atmosphere.[39−41] Important indicators of leaf status such as stoma
sizes and densities[42−44] have been monitored using leaves of S. aureus with leaf sensors attached for time periods
from 15 to 45 days. Leaf regions underneath and surrounding the sensors
have been categorized as the experimental group and the control group,
respectively. Figure a shows representative images of the experimental group (left) and
the control group (right) of a leaf after 15-day sensor attachment.
The growth of leaves leads to increased stoma sizes and decreased
stoma densities both in the experimental group and the control group,
as shown in Figures b,c as well as in Table S1. This phenomenon
accords well with the relationship between stoma sizes and densities
reported in previous paper.[45] It is noticeable
that both the length and the width have steadily increased with negligible
difference between the experimental groups and the control groups
(Figure b). However,
the experimental group exhibits a larger reduction in the stomata
density from 59.6 to 48.3 per mm2 as compared with only
a change of 2.8 per mm2 in the control group (Figure c). The preliminary
biological study has demonstrated that the fundamental functions of
leaves maintain unchanged during the extended measurement period over
45 days. The existence of the leaf sensors may have an only minimum
influence to the leaf growth as observed by the reduced stoma density.
Further investigation will be conducted to supply an in-depth understanding
of the mutual influence between leaves and leaf sensors.
Figure 5
Study of the
biological effect of the leaf sensor to hosting leaves.
(a) Images of stomas of the experimental group (left) and the control
group (right). Statistic results of changes in (b) stoma sizes and
(c) density of experimental and control groups in 45 days.
Study of the
biological effect of the leaf sensor to hosting leaves.
(a) Images of stomas of the experimental group (left) and the control
group (right). Statistic results of changes in (b) stoma sizes and
(c) density of experimental and control groups in 45 days.
Conclusions
Techniques for developing
multifunctional stretchable sensors for
continuous monitoring of long-term leaf physiology and microclimate
have been presented. A representative sensing system has been constructed
using ultrasoft and thin materials as well as stretchable structures,
allowing maximum adaptability to surface morphology of the leaves.
By introducing the island-bridge design with self-similar second-order
serpentine structures, the stretchability of the sensor can be enhanced
to match the growth of leaves, enabling unique capability for long-term
monitoring that is compared differently than other flexible leaf sensors.
In addition, multifunctional sensing elements offer the capability
to tailor functions of the sensors according to the demands of agriculture
production. The leaf sensor reshapes the appearance of agriculture
sensing by allowing people to synchronize plant growth with both intrinsic
and extrinsic conditions and advances both methodology and paradigm
of flexible electronics and agriculture sensors. Similar stretchable
sensors may be used to improve crop yield and quality through planning
and managing agriculture resources effectively, leading to higher
profits and sustainable agriculture. It is also feasible in the future
investigation to integrate other sensing elements to monitor developments
of plant diseases and insect pests, increasing the capability to prevent
and minimize the negative effect on agriculture production. Last,
these sensors may help to gain fundamental understandings of plant
growth in different environments and knowledge to mitigate adverse
environmental conditions for agriculture and forestry productions.
For practical use, the density of sensors depends on specific applications.
For small-scale botanical and biology studies in which precise physiological
and environmental conditions of each plant are need, the sensors may
be applied to each tested plant. In large-scale agricultural and industrial
production, each sensor may cover a relatively large area of crops
that are subjected to the same growth conditions. Several such sensors
may be used to conduct mapping of the growth conditions of crops over
large areas to obtain overall situation of the entire farmland. To
optimize the leaf sensor, higher-order serpentine structures could
be designed to improve the stretchability, and ultrathin elastomer
materials could be utilized in the flexible cable to release the constraint
on the sensor.
Experimental Section
Design of the Multifunctional
Leaf Sensor
The hydration
sensing element consists of an inner disk (120 μm in radius)
surrounded by an open-ended annulus (250 μm in inner radius
and 400 μm in outer radius), forming a planar capacitor whose
dielectric permittivity is determined by leaf hydration. The temperature
sensing element is made of an ultrathin copper film (thickness: 50
nm) patterned into a meander shape (width: 20μm) to achieve
large resistances (1.0 kΩ) compared to serpentine interconnections
(∼10 Ω). This sensing element is located in a neutral
mechanical plane between top and bottom PI membranes (length: 1100
μm, wide: 900 μm) to minimize strains caused by leaf growth.
Strain sensing elements contain two perpendicular strips (500 μm
in length and 30 μm in width) made of single-walled CNTs (SWCNTs)
and respond uniaxial strain induced by mechanical deformation because
of leaf growth. The ambient light illuminance is measured by a SU-8
encapsulated phototransistor (1100 × 1100 × 30 μm3). The SU-8 encapsulation facilities assembly and interconnection
of the phototransistor with the pre-defined copper electrodes on the
leaf sensor and protects the thinned phototransistor from cracking.
All elements are connected with screen-printed flexible Ag cables
with a line width of 750 μm.
Thinning and Encapsulation
of the Phototransistor
A
bare die phototransistor (ST-0128, Opto Tech Corp.) was mechanically
thinned using a grinding machine (UNIPOL-802, MTI Corp.) for 6 h,
resulting in a reduction of thickness from 200 μm to approximately
20 μm to enable intimate contact with the leaf. As shown in Figure S4, the thin-film phototransistor was
then transfer printed onto an uncured PI film on a sacrificial polymethyl
methacrylate (PMMA, 950 PMMA A4, MicroChem Corp.) layer on a glass
substrate. The PI film was then cured in a vacuum oven at 250 °C
for 2 h. A layer of SU-8 (SU-8 2015, MicroChem Corp.) with a thickness
of 25 μm was spin-coated and patterned to expose the emitter
of the phototransistor and form a square encapsulation layer (1100
× 1100 μm2) that encloses the phototransistor.
Magnetron sputtering and patterning of stacked layers of Ti/Cu/Ti/Au
(5/500/5/50 nm) created interconnection between the emitter and the
pre-defined electrode on the leaf sensor. Plasma etching of the PI
film exposed the sacrificial PMMA, allowing releasing of packaged
phototransistor through dissolving the PMMA in acetone. Finally, the
PI film on the backside of the phototransistor was completely removed
by plasma etching to complete the encapsulation process.
Fabrication
of the Multifunctional Sensor
The fabrication
process of a multifunctional leaf sensor started with spin-coating
a layer of PI (1 μm in thickness) onto a copper foil (3 μm
in thickness) (Figure S5). The PI-coated
Cu foil was laminated onto a glass slide coating with PDMS (Sylgard
184, Dow Corning Corp.). The copper film was patterned into the hydration
sensing element as well as serpentine interconnects, followed by coating
an additional PI film to form an insulating layer. Plasma etching
opened vias for electrical contact with the subsequent metallization
layer on the PI film, followed by coating and patterning of Ti/Cu
layers (2 nm/50 nm) to form the temperature sensing element. A third
PI insulating layer was coated and etched to form vias, which allowed
connection between drop-casted SWCNTs (1 μL aqueous dispersion,
TNSR, Chengdu Organic Chemicals Co., Ltd.) with the serpentine interconnects.
A final PI layer was then applied and patterned by plasma to complete
the fabrication process. A water-soluble cellulose tape (ASWT-2, Aquasol
Corp.) allowed picking up the resulting sensor from the PDMS substrate
and transfer-printing the sensor onto a porous silicone elastomer
membrane (Silbione RT GEL 4717 A&B, China National Bluestar (Group)
Co., Ltd). Finally, a packaged phototransistor was transferred and
electrically connected with the leaf sensor with silver epoxy (8000H,
Shenzhen Sunflower Electronic Materials Co., Ltd.).
Multifunctional
Wireless Sensing Circuit
The multifunctional
wireless sensing circuit contains stacked layers of circuit boards
(Figure S2). The impedance of the hydration
sensing element was measured by an impedance converter (AD5933, Analog
Devices Inc.), which supplied an input voltage at frequencies from
20 to 100 kHz and measured the magnitude and the phase of the return
voltage. A bridge circuit connected with the temperature sensing element
and converted resistance changes to voltage changes (Figure S6a). The strain sensing element was connected into
a bridge circuit, which effectively eliminated influence from the
temperature to the resistance (Figure S6b). The sensing circuit for the phototransistor supplied a voltage
of 3.3 V to the collector of the phototransistor. The light-dependent
collector-emitter current was converted into voltage values through
a load resistance. A microcontroller (MCU, LPC1114, NXP Semiconductors
Corp.) communicated with AD5933 via the I2C serial interface protocol
and acquired signals of temperature, ambient light, and strain through
three internal 10-bits analogue-to-digital converters. The digitalized
data were packed into data packages and sent to a remote receiver
connected with a computer through Zigbee (XBee-PRO S3B 900HP, Digi
International Inc.). The bottom PCB managed power supplied by either
a rechargeable battery or external power supply. The rechargeable
battery had a capacity of 370 mAh, allowing continuous operation for
7 h under 165 mW/h power consumption. The middle PCB contained signal
acquisition circuits as well as flexible cable connecting pads to
allow connection with flexible cables. The top PCB mainly contained
the MCU and the Zigbee module, which used a frequency band from 902
to 928 MHz to communicate with a remoted Zigbee module that was connected
to a computer for data storage and display.
Finite Element Simulation
A FEA software ABAQUS was
used to investigate the mechanical deformation of the sensor under
stretching. Young’s moduli of Silbione, PI, Cu, Au, and CNT
were set as 0.01, 2500, 119 000, 79 000, and 395 000
MPa, respectively. The Poisson’s ratio is 0.49 for Silbione
and PI, 0.34 for Cu, 0.44 for Au, and 0.285 for CNT. Considering the
small thickness of sensing elements and connections, they were modeled
as skin layers on the surface of substrates to reduce computational
load. Various composite material properties were assigned to the skin
layers, depending on the location. For example, the central region
of serpentine interconnects is a multilayer structure of PI/Cu/PI.
Meanwhile, it is reasonable to assume that connections between the
four sensing elements are very weak because of the softness of substrates.
Displacement boundary conditions were imposed to stretch the sensor
by 150% along the y-direction and 60% along the x-direction.
Study of Mutual Influence between the Sensor
and the Leaf
Leaves of the experimental group and the control
group were cut
into 1.5 × 1.5 cm2 samples for the stomatal morphology
analysis. The samples were immersed in sodium hypochlorite 20% at
30 °C for 1 h, followed by water rinsing. Epidermis and mesophylls
of the samples were then segregated under an optical microscope (ST60,
Sunny Optical Technology Co., Ltd.). The epidermis was stained in
safranin for 5 min and dehydrated in ethanol. All images were captured
through a microscope (VHX-1000, Keyence Corp.) at ×500 magnification
(0.3185 mm–2 fields of view). The experimental group
and the control group were taken at different times each contains
10 images. Stoma sizes and density were counted for all images with
ImageJ.
Authors: Pavlo Gordiichuk; Sarah Coleman; Ge Zhang; Matthias Kuehne; Tedrick T S Lew; Minkyung Park; Jianqiao Cui; Allan M Brooks; Karaghen Hudson; Anne M Graziano; Daniel J M Marshall; Zain Karsan; Sheila Kennedy; Michael S Strano Journal: Sci Adv Date: 2021-09-08 Impact factor: 14.136