Supplementary Materials for...The silicon p-n diode on the SOI wafer was transferred onto the target...
Transcript of Supplementary Materials for...The silicon p-n diode on the SOI wafer was transferred onto the target...
advances.sciencemag.org/cgi/content/full/4/1/eaap9841/DC1
Supplementary Materials for
Soft, smart contact lenses with integrations of wireless circuits, glucose
sensors, and displays
Jihun Park, Joohee Kim, So-Yun Kim, Woon Hyung Cheong, Jiuk Jang, Young-Geun Park, Kyungmin Na,
Yun-Tae Kim, Jun Hyuk Heo, Chang Young Lee, Jung Heon Lee, Franklin Bien, Jang-Ung Park
Published 24 January 2018, Sci. Adv. 4, eaap9841 (2018)
DOI: 10.1126/sciadv.aap9841
The PDF file includes:
Supplementary Materials and Methods
fig. S1. Fabrication processing steps of the hybrid substrate.
fig. S2. AFM data analysis.
fig. S3. Optical transmittance (black) and haze (red) spectra of the silicone
elastomeric film.
fig. S4. The variation of optical properties against mechanical stretching of the
hybrid substrate (from 0 to 30% in tensile strain).
fig. S5. Original image for the photograph test to identify the clarity of hybrid
substrate.
fig. S6. Wireless display circuit composed of an antenna, a rectifier, and an LED
pixel.
fig. S7. Fabrication procedures of wireless display on the hybrid substrate.
fig. S8. Characteristics of the stretchable, transparent AgNF electrode as antenna.
fig. S9. Characteristics of the Si diode and SiO2 capacitor.
fig. S10. Sequential schematic images to transform to the lens shape.
fig. S11. Mechanism of glucose sensing on graphene channel.
fig. S12. The magnified real-time sensing result (at the first detection of glucose
level) to verify the response time.
fig. S13. Stability of the smart contact lens system.
fig. S14. The relationship between the glucose concentration and luminance of the
LED.
fig. S15. SAR simulation result.
table S1. Comparison with other noninvasive glucose monitoring technologies.
Legends for movies S1 to S4
References (43–45)
Other Supplementary Material for this manuscript includes the following:
(available at advances.sciencemag.org/cgi/content/full/4/1/eaap9841/DC1)
movie S1 (.mp4 format). Embedding procedure of the hybrid substrate in the
contact lens.
movie S2 (.mp4 format). Wireless operation of wireless display with lens shape.
movie S3 (.mp4 format). In vivo test of soft, smart contact lens for wireless
operation.
movie S4 (.mp4 format). In vivo test of soft, smart contact lens for heat
generation test.
Supplementary Materials and Methods
Preparation of the rectifier
The process began by defining p- and n-doped regions on SOI wafer (Soitec, unibond with 300 nm top
p-type Si layer with the resistivity of 14-22 Ω·cm and 400 nm-thick buried oxide layer) via impurity
diffusion. Boron was pre-deposited in the furnace at the temperature of 1,050 °C for 70 sec under the
flow of N2 (1,000 sccm) using RTA to diffuse the boron concentration uniformly across the 300 nm-
thick top silicon wafer. After photo-lithographically patterning the SiO2 (thickness: 300 nm) deposited
by PECVD on the p-doped area, phosphorus was deposited in the RTA furnace at 1,050 °C for 120 sec
under the flow of N2 (1,000 sccm) in order to convert p-type into n-type. Subsequently, the SiO2 and
SiOx on the surface were removed using buffered HF solution. The silicon p-n diode on the SOI wafer
was transferred onto the target substrate system (500 nm-thick parylene/800 nm-thick Cu film/Si wafer)
by etching away the buried oxide layer of SOI wafer with 50% HF solution, and then picking up the Si
diode with PDMS stamp. After transfer, anode and cathode (Cr/Au: 3/100 nm) of diode were deposited
and patterned photolithographically. After that, the capacitor for rectifier was manufactured. In the
capacitor, the bottom electrode is connected to the cathode (n-type side of the diode), and the 300 nm-
thick SiO2, dielectric material for capacitance, is deposited by PECVD. The top electrode of the
capacitor (Cr/Au: 3/100 nm) was also deposited and patterned.
Fabrication of AgNF electrodes for antenna and interconnects
In order to form ultra-long AgNFs, a suspension of Ag nanoparticles (NPK, Korea, average diameter: 40
± 5 nm, solvent: ethylene glycol, concentration = 50 wt.%) was electrospun continuously onto the target
substrate. Then, the electrospun sample was thermally annealed at 150 °C for 30 min to coalesce the Ag
nanoparticles into electrically-conductive AgNFs with an average diameter of 338 ± 35 nm, and these
annealed AgNFs were photolithographically patterned using wet etching process for the antenna and
interconnects.
Graphene synthesis using chemical vapor deposition (CVD) and transfer of graphene on the target
substrate
A Cu foil (Alfa Aesar, item No.: 13382) on a quartz stage was placed in the center of quartz CVD
chamber under low vacuum condition (10 mTorr). After loading, the furnace was heated up to 1,000 °C
under the flow of Ar (200 sccm) and H2 (500 sccm). Under the flow of CH4 (12 sccm) and H2 (500
sccm), the graphene synthesis was carried out for 5 min, and then the furnace was cooled rapidly to
room temperature with flowing Ar (500 sccm). A 200 nm thickness of poly(methyl methacrylate)
(PMMA, Microchem Corp., 950 PMMA) was spun on the graphene sample which is synthesized on the
Cu foil as a supporting layer. The metal foil was removed by floating on a diluted etching solution of
FeCl3: HCl: H2O (1:1:20 vol.%). After the etching process, the PMMA coated graphene layer was
floated onto the deionized water for rinsing. Subsequently, the sample was transferred onto the target
substrate, and the transferred sample was dried in the atmosphere for 4 hours. After drying, the PMMA
layer was dissolved by acetone.
Electrical characterization
The four-point probe method was used for the measurement of sheet resistance using a probe station
with a Keithley 4200-SCS semiconductor parametric analyzer. The electrical characteristics of Si diodes
and real-time sensing of glucose sensor were conducted using a probe station (Keithley 4200-SCS). (i)
The I-V curves of Si diodes were measured with the drain bias (VD) from -5 V to 5 V. (ii) The real-time
sensing of glucose sensor was conducted with the VD of 5 V.
Wireless measurements and operations
For wireless operations of wireless display and soft, smart contact lens, the power is generated and
wirelessly transmitted by the waveform generator (Keysight 33520B) connected with RF power
amplifier (A-300). The transmitted waveform is measured by the oscilloscope (Keysight MSOX3032T).
Thermal characterization
For the thermal characterization during in-vivo test, the temperature was measured by an LWIR camera
(T650sc, FLIR Systems, Wilsonille, OR, USA). The temperature distribution of images and video was
analyzed using the FLIR ResearchIR software (Research IR Max, FLIR Systems).
fig. S1. Fabrication processing steps of the hybrid substrate.
fig. S2. AFM data analysis. SEM image (left) shows the scanned location on the hybrid substrate.
Scale bar, 500 μm. The height profile (right) of AFM image (green line in Fig. 2D) shows negligible
height difference.
fig. S3. Optical transmittance (black) and haze (red) spectra of the silicone elastomeric film.
fig. S4. The variation of optical properties against mechanical stretching of the hybrid substrate
(from 0 to 30% in tensile strain).
fig. S5. Original image for the photograph test to identify the clarity of hybrid substrate.
fig. S6. Wireless display circuit composed of an antenna, a rectifier, and an LED pixel. The
rectifier converts the AC signal induced in the antenna into the DC, and the DC powers the LED pixel
which is connected to the rectifier in parallel.
fig. S7. Fabrication procedures of wireless display on the hybrid substrate.
fig. S8. Characteristics of the stretchable, transparent AgNF electrode as antenna. (A) Sheet
resistance and optical transmittance of the AgNF films as function of area fraction. (B) Relative
change in resistance of AgNF films as a function of strain. (C) Power transmission efficiency of the
AgNF antenna as a function of frequency. (D) Transmitted voltage of the AgNF antenna as a function
of frequency.
fig. S9. Characteristics of the Si diode and SiO2 capacitor. (A) Optical microscopic image of
rectifier. Scale bar, 200 μm. (B) Characteristics of the Si diode. (C) Characteristics of the SiO2
capacitor.
fig. S10. Sequential schematic images to transform to the lens shape. The circuit in the hybrid
substrate was cut off with donut shape. The circuit was located inside the lens mold, and then the
contact lens material is fulfilled. After pressing the upper mold with 313 kPa, followed by curing
process, the circuit is embedded into the contact lens.
fig. S11. Mechanism of glucose sensing on graphene channel. When the glucose approaches to the
functionalized graphene channel. The GOD will convert glucose into gluconic acid in producing a
byproduct, H2O2. After that, H2O2 will be naturally decomposed into O2, electron, proton (H+ ion). In
addition, the protons will increase the major carrier density of graphene channel.
fig. S12. The magnified real-time sensing result (at the first detection of glucose level) to verify the
response time.
fig. S13. Stability of the smart contact lens system. (A) Calibration curves for various glucose
concentrations with the passage of time in artificial tear fluid. (B) Relative change in the rectified
voltages of wirelessly transmitted power as a function of the storage time in artificial tear fluid. (C)
The relative change in luminance as a function of the stretching and releasing cycles (tensile strain of
30%).
fig. S14. The relationship between the glucose concentration and luminance of the LED.
fig. S15. SAR simulation result. The transmitting power sets as 50 W for the extreme environment
test.
table S1. Comparison with other noninvasive glucose monitoring technologies.
Type of
body fluid Type of sensor Method to display results Ref.
Tear Resistive-type RF signal (reflectance, S11) 14
Sweat Electrochemical-
type
Connection with smartphone by
Bluetooth 43
Sweat Colorimetric-type Colorimetric method and NFC
connection for quantitation 44
Saliva Electrochemical-
type
Wireless communication with
customized module (computer) 45
movie S1. Embedding procedure of the hybrid substrate in the contact lens.
movie S2. Wireless operation of wireless display with lens shape.
movie S3. In vivo test of soft, smart contact lens for wireless operation.
movie S4. In vivo test of soft, smart contact lens for heat generation test.