Method for measurement of the density of thin films of small organic molecules

An accurate and sensitive method is reported to measure the thin-film density of vacuum-deposited, small-molecular organic semiconductor materials. A spectrophotometer and surface profiler had been used to determine the mass and thickness of organic thin film, respectively. The calculated density of tris-(8-hydroxyquinolato) aluminum (Alq(3)) thin film was 1.31+/-0.01 gcm(3). Vacuum pressures and thin-film growth rates are found to have less impact on the thin-film density of organic material. However, the thin-film density of organic material strongly depends on its chemical structure and molecular weight. Specifically, the chemical structure determines the density of organic material that affects the molecular volume and intermolecular stacking.     

Fully automated measurement setup for non-destructive characterization of thermoelectric materials near room temperature

A measurement setup is presented that allows for a complete and non-destructive material characterization of electrochemically deposited thermoelectric material. All electrical (Seebeck coefficient α, electrical conductivity σ), thermal (thermal conductivity λ), and thermoelectric (figure of merit ZT) material parameters are determined within a single measurement run. The setup is capable of characterizing individual electrochemically deposited Bi(2+x)Te(3-x) pillars of various size and thickness down to a few 10 μm, embedded in a polymer matrix with a maximum measurement area of 1 × 1 cm(2). The temperature range is limited to an application specific window near room temperature of 10?°C to 70?°C. A maximum thermal flux of 1 W∕cm(2) can be applied to the device under test (DUT) by the Peltier element driven heat source and sink. The setup has a highly symmetric design and DUTs can be mounted and dismounted within few seconds. A novel in situ recalibration method for a simple, quick and more accurate calibration of all sensors has been developed. Thermal losses within the setup are analysed and are mathematically considered for each measurement. All random and systematic errors are encountered for by a MATLAB routine, calculating all the target parameters and their uncertainties. The setup provides a measurement accuracy of ±2.34 μV∕K for α, ±810.16 S∕m for σ, ±0.13 W∕mK for λ, and ±0.0075 for ZT at a mean temperature of 42.5?°C for the specifically designed test samples with a pillar diameter of 696 μm and thickness of 134 μm, embedded in a polyethylene terephthalate polymer matrix.     

Effects of morphological control on the characteristics of vertical-type OTFTs using Alq3

We have fabricated vertical-type organic thin-film transistors (OTFTs) using tris-(8-hydroxyquinoline) aluminum (Alq(3)) as an n-type active material. Vertical-type OTFT using Alq(3) has a layered structure of Al(source electrode)/Alq(3)(active layer)/Al(gate electrode)/Alq(3)(active layer)/ITO glass(drain electrode). Alq(3) thin films containing various surface morphologies could be obtained by the control of evaporation rate and substrate temperature. The effects of the morphological control of Alq(3) thin layer on the grain size and the flatness of film surface were investigated. The characteristics of vertical-type OTFT significantly influenced the growth condition of Alq(3) layer.     

Ultrahigh vacuum-compatible fabrication and electrical characterization systems for environmentally sensitive metal oxide semiconductor capacitors

We describe an integrated, ultrahigh vacuum system for metal oxide semiconductor (MOS) device fabrication and characterization. This system is advantageous for electrical property measurements on electronic devices with environmentally sensitive materials and is especially important as device dimensions approach the nanoscale. Without exposure to atmosphere, MOS capacitors were fabricated by evaporatively depositing gate metal on molecular-beam-epitaxy (MBE) grown dielectrics through a shadow mask in an UHV electrode-patterning chamber. Finished devices were transferred in UHV to an in situ UHV electrical characterization probe station. We obtained excellent agreement between air-ambient ex situ and in situ probe station measurements with less than 0.3% systemic error for frequencies from 20 Hz to 1 MHz. We have successfully measured MOS capacitors with sensitivity to a density of interface states of 1x10(10) states cm(-2) eV(-1). These measurements show 0.5% systematic error for measurement frequencies from 20 Hz to 1 kHz and less than 0.1% from 1 kHz to 1 MHz. The integrated system presented here is one where complex, MBE-grown MOS heterostructures can be synthesized and tested rapidly to explore new field-effect-device physics and functionality.     

High temperature Z-meter setup for characterizing thermoelectric material under large temperature gradient

To properly estimate a thermoelectric material's performance, one should be able to characterize a single thermoelectric (TE) element with a large temperature gradient. In this work, we present an experimental setup including a Z-meter that can heat the sample to a very high temperature of 1200 °C in vacuum. The Z-meter can simultaneously measure all three thermoelectric parameters (Seebeck coefficient, thermal conductivity, and electrical conductivity), as well as measure the generated power and the efficiency for a single TE leg. Furthermore, this measurement of power conversion efficiency is used to generate a measure of the material's ZT. An in situ metallurgical bond was used to achieve low thermal (0.05 Kcm(2)∕W) and electrical (3 mΩ) contact parasitics. An integrated strain gauge ensures reproducible thermal contact. At high temperature (>600 K), radiative heat transfer is modeled and the instrument is optimized to suppress the systematic error to below 7%. The TE parameters and ZT for a bulk-sample (Bi(2)Te(3)) and a thin-film sample (ErAs:InGaAlAs) with a large temperature gradient (ΔT ～ 200 K) have been measured and are within 3%-7% of the independently measured values.     

Effects of morphological control on the characteristics of vertical-type OTFTs using Alq3

We have fabricated vertical-type organic thin-film transistors (OTFTs) using tris-(8-hydroxyquinoline) aluminum (Alq₃) as an n-type active material. Vertical-type OTFT using Alq₃ has a layered structure of Al(source electrode)/Alq₃(active layer)/Al(gate electrode)/Alq₃(active layer)/ITO glass(drain electrode). Alq₃ thin films containing various surface morphologies could be obtained by the control of evaporation rate and substrate temperature. The effects of the morphological control of Alq₃ thin layer on the grain size and the flatness of film surface were investigated. The characteristics of vertical-type OTFT significantly influenced the growth condition of Alq₃ layer.     

Direct writing of nanomaterials for flexible thin-film transistors (fTFTs)

This paper focuses on the utilization of carbon nanotubes for the fabrication of thin-film transistors (TFTs) using a direct-write inkjet process. Single-walled carbon nanotubes (SWNTs) are well regarded for their superior electrical, magnetic, and thermal properties. The development of TFTs requires high carrier mobility comparable to that of SWNTs (100,000 cm²/V.s) which can be doped as both n- and p-types. We have enriched semiconducting SWNTs (s-SWNTs) into specific chiralities to provide a consistent band gap required for the fabrication of transistors with reproducible electrical properties. In this research, we investigate the use of direct-write inkjet to deposit enriched s-SWNTs on Kapton substrates to fabricate flexible thin-film transistors (fTFTs). The direct writing technique provides accurate deposition control and reproducibility to print s-SWNTs over large areas. Optical and atomic force microscopy images identify threshold of nanotube bundle connectivity for different deposition configurations. We demonstrate the fabrication of SWNT traces with varying conductivity and transport characteristics towards large-scale fTFTs.     

A combined scanning tunneling microscope-atomic layer deposition tool

We have built a combined scanning tunneling microscope-atomic layer deposition (STM-ALD) tool that performs in situ imaging of deposition. It operates from room temperature up to 200 °C, and at pressures from 1 × 10(-6) Torr to 1 × 10(-2) Torr. The STM-ALD system has a complete passive vibration isolation system that counteracts both seismic and acoustic excitations. The instrument can be used as an observation tool to monitor the initial growth phases of ALD in situ, as well as a nanofabrication tool by applying an electric field with the tip to laterally pattern deposition. In this paper, we describe the design of the tool and demonstrate its capability for atomic resolution STM imaging, atomic layer deposition, and the combination of the two techniques for in situ characterization of deposition.     

Vector control of induced magnetic anisotropy using an in situ quadrupole electromagnet in ultrahigh vacuum sputtering

We demonstrate the incorporation of a quadrupole electromagnet into an ultrahigh vacuum sputtering system for the vector control of induced magnetic anisotropy in magnetic thin-film heterostructures. A stationary quadrupole electromagnet is used to generate a magnetic field, which rotates synchronously with the physical axes of the substrate in situ during sputtering. An arbitrary anisotropy direction can be set for successive ferromagnetic layers by adjusting the phase difference of substrate and field rotation. The ability to rotate the substrate during deposition and change anisotropy without breaking vacuum enables the deposition of magnetically soft heterostructures with arbitrary in-plane anisotropy axes.     

Evolution of film curvature profile during light-emitting diode epitaxial growth

Wafer bowing control is critical to improve epitaxial growth quality, especially for large wafers inside a metal–organic chemical vapor deposition reactor. An in-situ monitoring system was developed for real-time characterization of curvature mapping and epitaxial layer reflectance and temperature. Using deflectometry with parallel laser beams and position detector arrays, simultaneous curvature scans were conducted in two perpendicular directions over 4-in wafers. The developed system eliminated the effect of vibrations. Growth transients and curvature mappings are presented for the stages of epitaxial growth. Thermal and thickness gradient effects were analyzed to explain aspherical bowing. This technique appears suitable for closed-loop process optimization during light-emitting diode growth and other epitaxial growth processes.     

The flexible Ca-test: an improved performance in a gas permeability measurement system

A flexible performance permeability measuring test for flexible organic light-emitting diodes is described in this paper. A single thin film layer of gas barriers is constructed on polyethersulfone (PES). The barrier coats the upper and lower surfaces of the PES layer. Two PES samples, one coated with Al(2)O(3) on both surfaces and the other coated on a single surface, were made for comparison. According to this test, the time-dependent transmission curve of the one sided barrier sample had a linear slope which measured 1.65 g∕m(2)∕day at room temperature at a 50% relative humidity. This result shows that the measurement time is about 182% faster than has been achieved with the conventional test structure that uses a glass substrate. In addition, this measurement structure not only reduces the inevitable electrical noise which occurs during measurement but also increases the water vapor permeation signal. These effects improve the sensing reliability of the test. In addition, this structure is flexible, so one can instantly detect barrier performance changes when applying external stress.     

Real-time thermal characterization of 12 nl fluid samples in a microchannel

This work presents a novel method and a device for real-time simultaneous measurement of the thermal conductivity and heat capacity of 12 nl fluid samples. The device uses a micromachined thermal sensor composed of a microchannel and a thin-film probe. The method, based on the 3 omega technique, employs a multiparameter-fitting scheme to determine the thermal properties with numerical computation of heat transfer. The thermal properties of 12 nl samples have been measured successfully by the sensor. Furthermore, real-time thermal characterization of fluid samples flowing in a microchannel has been demonstrated, manifesting strong potential of the proposed technique as an in situ probe in various microfluidic applications.     

Note: Heated sample platform for in situ temperature-programmed XPS

We present the design, fabrication, and performance of the multi-specimen heated platform for linear in situ heating during the Temperature-Programmed XPS (TPXPS). The platform is versatile, compatible with high vacuum (HV) and bakeout. The heater platform is tested under in situ linear heating of typical high surface area sorbent∕catalyst support--nanoporous TiO(2). The platform allows the TPXPS of multiple samples located on specimen disk that can be transferred in and out of the TPXPS chamber. Electric characteristics, temperature and pressure curves are provided. Heating power supply, PID temperature controller, data-logging hardware and software are described.     

Real-time measurement system for tracking birefringence, weight, thickness, and surface temperature during drying of solution cast coatings and films

This paper describes the design and performance of a new instrument to track temporal changes in physical parameters during the drying behavior of solutions, as well as curing of monomers. This real-time instrument follows in-plane and out-of-plane birefringence, weight, thickness, and surface temperature during the course of solidification of coatings and films through solvent evaporation and thermal or photocuring in a controlled atmosphere. It is specifically designed to simulate behavior of polymer solutions inside an industrial size, continuous roll-to-roll solution casting line and other coating operations where resins are subjected to ultraviolet (UV) curing from monomer precursors. Controlled processing parameters include air speed, temperature, initial cast thickness, and solute concentration, while measured parameters are thickness, weight, film temperature, in-plane and out-of-plane birefringence. In this paper, we illustrate the utility of this instrument with solution cast and dried poly (amide-imide)∕DMAc (Dimethylacetamide) solution, water based black paint, and organo-modified clay∕NMP (N-Methylpyrrolidone) solution. In addition, the physical changes that take place during UV photo polymerization of a monomer are tracked. This instrument is designed to be generic and it can be used for tracking any drying∕swelling∕solidification systems including paper, foodstuffs such as; grains, milk as well as pharmaceutical thin paste and slurries.     

C-V measurements of micron diameter metal-oxide-semiconductor capacitors using a scanning-electron-microscope-based nanoprobe

The C-V electrical characterization of microstructures on a standard probe station is limited by the magnification of the imaging system and the precision of the probe manipulators. To overcome these limitations, we examine the combination of in situ electrical probing and a dual column scanning electron microscope/focused ion beam system. The imaging parameters and probing procedures are carefully chosen to reduce e-beam damage to the metal oxide semiconductor capacitor device under test. Estimation of shunt capacitance is critical when making femtofarad level measurements. C-V measurements of micron size metal-oxide-silicon capacitors are demonstrated.     

IMPACT: a facility to study the interaction of low-energy intense particle beams with dynamic heterogeneous surfaces

The Interaction of Materials with Particles and Components Testing (IMPACT) experimental facility is furnished with multiple ion sources and in situ diagnostics to study the modification of surfaces undergoing physical, chemical, and electronic changes during exposure to energetic particle beams. Ion beams with energies in the range between 20 and 5000 eV can bombard samples at flux levels in the range of 10(10)-10(15) cm(-2) s(-1); parameters such as ion angle of incidence and exposed area are also controllable during the experiment. IMPACT has diagnostics that allow full characterization of the beam, including a Faraday cup, a beam imaging system, and a retarding field energy analyzer. IMPACT is equipped with multiple diagnostics, such as electron (Auger, photoelectron) and ion scattering spectroscopies that allow different probing depths of the sample to monitor compositional changes in multicomponent and/or layered targets. A unique real-time erosion diagnostic based on a dual quartz crystal microbalance measures deposition from an eroding surface with rates smaller than 0.01 nm/s, which can be converted to a sputter yield measurement. The monitoring crystal can be rotated and placed in the target position so that the deposited material on the quartz crystal oscillator surface can be characterized without transfer outside of the vacuum chamber.     

脉冲激光溅射沉积技术的发展及其应用研究

薄膜材料已经在半导体材料、超导材料、生物材料等方面得到广泛应用.为了得到高质量的薄膜材料,脉冲激光溅射沉积(PLD)技术受到了广泛的关注.文中介绍了脉冲激光溅射沉积薄膜的基本原理及特点,分析了脉冲激光溅射沉积技术在制备高温超导膜、铁电薄膜、生物陶瓷薄膜等功能薄膜方面的应用研究.大量研究表明,脉冲激光溅射沉积是目前最好的...     

Design of a physical vapor transport cell for time controlled deposition of nucleation phase organic thin films

A portable high vacuum chamber has been designed to implement a solenoid operated shutter used as a substrate cache during short duration deposition of organic thin films via the physical vapor transport (PVT) method. This PVT cell was designed for the study of gravity effects on nucleation phase organic thin films obtained in laboratory unit g conditions and especially low g conditions found onboard parabolic flights. The design challenges met were, notably, the timely control of deposition on the substrate during parabolas and maintenance of the experimental cell pressure during operation of the shutter. Nucleation phase thin films of the organic hole transporting semiconductor N,N' -bis(3-methylphenyl)-N,N' -bis(phenyl)benzidine (TPD), obtained with the use of the PVT cells, show that the moving shutter has an effect on the convective PVT gas flow; however, as convection is reduced, this effect is observed to be equally reduced.     

Broad-band and high-temperature ultrasonic transducer fabricated using a Pb(In(1∕2)Nb(1∕2))-Pb(Mg(1∕3)Nb(2∕3))-PbTiO3 single crystal∕epoxy 1-3 composite

In this paper, 1-3 composites based on Pb(In(1∕2)Nb(1∕2))-Pb(Mg(1∕3)Nb(2∕3))-PbTiO(3) (PIMNT) single crystal and high-temperature epoxy were fabricated with various volume fractions of PIMNT single crystal ranging from 0.4 to 0.9. The electrical properties were studied as functions of PIMNT volume fraction and temperature, and it revealed that the nature of ultrahigh electromechanical coupling coefficient (0.82-0.93) and low acoustic impedance (17-19 MRayl) of the composites can be retained within a wide temperature range from room temperature to 185?°C. Single element ultrasonic transducer using the PIMNT 1-3 composite was fabricated and characterized as a function of temperature. It was found that the transducer can still work normally at high temperatures, such as 165?°C, possessing a bandwidth of 95% and insertion loss of -27 dB.     

Isochoric heating of foamed metal using pulsed power discharge as a making technique of warm dense matter

To generate well-defined warm dense state for evaluating electrical conductivity by using pulsed-power discharge, we have proposed an isochoric heating of foamed metal. Isochoric heating can be achieved by surrounding the foamed metal with a rigid-walled sapphire capillary. We evaluate the temperature and electrical conductivity of the foam∕plasma based on the line-pair method of the foam∕plasma emission and on the voltage-current waveforms. The electrical conductivity observed agrees with previous experiments and predictions. Thus, the proposed technique yields the electrical conductivity of warm dense matter with a well-defined temperature.