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Cross-sectional Kelvin probe force microscopy on III–V epitaxial multilayer stacks: challenges and perspectives

The development of photovoltaic (PV) technologies has progressed significantly over the past twenty years as a result of considerable advancements in solar cell device engineering and material science. *

As a consequence, solar cells have turned into complex structures containing numerous layers and interfaces. The capability to conduct local investigations at the nanoscale level that provide information on the electrical properties of materials and along physical interfaces is becoming crucial for solar photovoltaic device efficiency improvement. *

The capability to conduct local investigations at the nanoscale level that provide information on the electrical properties of materials and along physical interfaces is becoming crucial for solar photovoltaic device efficiency improvement. *

Multilayer III–V-based solar cells are complex devices consisting of many layers and interfaces. *

The study and the comprehension of the mechanisms that take place at the interfaces is crucial for efficiency improvement. *

Electrical measurements based on scanning probe microscopy (SPM) allow for the analysis of two-dimensional (2D) features at the surface and along a physical cross section of nanoscale semiconductor structures. *

Among the wide variety of SPM techniques available, Kelvin probe force microscopy (KPFM) is an application of the atomic force microscope (AFM) for the evaluation of the surface potential with nanometric resolution. KPFM is a valuable investigative approach for the study of work functions via the measurement of the contact potential difference VCPD, that is, the difference between the electrostatic potential at the surface of the investigated structure and that of the KPFM probe. *

In the article “Cross-sectional Kelvin probe force microscopy on III–V epitaxial multilayer stacks: challenges and perspectives” Mattia da Lisca, José Alvarez, James P. Connolly, Nicolas Vaissiere, Karim Mekhazni, Jean Decobert and Jean-Paul Kleider apply frequency-modulated Kelvin probe force microscopy (FM-KPFM) under ambient conditions to investigate the capability of this technique for the analysis of an InP/GaInAs(P) multilayer stack. *

KPFM reveals a strong dependence on the local doping concentration, allowing for the detection of the surface potential of layers with a resolution as low as 20 nm. *

The analysis of the surface potential allowed for the identification of space charge regions and, thus, the presence of several junctions along the stack. Furthermore, a contrast enhancement in the surface potential image was observed when KPFM was performed under illumination, which is analysed in terms of the reduction of surface band bending induced by surface defects by photogenerated carrier distributions. The analysis of the KPFM data was assisted by means of theoretical modelling simulating the energy bands profile and KPFM measurements. *

KPFM was performed using a scanning probe microscopy system under ambient conditions and operated in the frequency-modulated KPFM (FM-KPFM) mode using a two-pass scanning mode, where the second pass was performed at a constant distance of 10 nm from the sample surface. *

The FM-KPFM mode was chosen over the amplitude-modulation mode (AM-KPFM) since it is well known that it provides better spatial resolution. In particular, in AM-KPFM the electrical force between the tip and the sample is directly evaluated, whereas in FM-KPFM the gradient of the force is analysed. As a result, FM-KPFM is more sensitive to local tip apex–sample surface interactions; therefore, long-range electrostatic interactions of the cantilever are reduced, as well as the effect of parasitic capacitances. Additionally, in FM-KPFM, surface potential measurements are less dependent on the lift-height tip–sample distance than in AM-KPFM since this mode is less sensitive to static offsets induced by capacitive coupling or crosstalk. *

The laser beam deflection system in the author’s AFM employs a laser wavelength of 1310 nm, which is well below the bandgap of the sample; therefore, the parasitic laser absorption, which may interfere with the KPFM measurement, is reduced to negligible levels. Highly doped NanoWorld n+-Si ARROW-EFM tips (typical AFM tip radius < 25 nm) with a conductive Pt/Ir coating at a typical resonance frequency of 75 kHz were used. *

Figure 4 from “Cross-sectional Kelvin probe force microscopy on III–V epitaxial multilayer stacks: challenges and perspectives” by Mattia da Lisca et al :
KPFM measurement under ambient conditions on the surface cross section of the sample under illumination: (a) topography and (b) VCPD image. A vertical coloured bar is included to ease the identification of the different layers. The profile in (c) corresponds to the region identified by the dotted white segments in (b), each point of the profile (vertical) direction being an average of 207 points over a width of 0.7 μm along the x axis. Several regions along the structure have been highlighted using different colours (see text). The black arrow indicates the space charge region at the InP:nid/InP:Zn interface.

*Mattia da Lisca, José Alvarez, James P. Connolly, Nicolas Vaissiere, Karim Mekhazni, Jean Decobert and Jean-Paul Kleider
Cross-sectional Kelvin probe force microscopy on III–V epitaxial multilayer stacks: challenges and perspectives
Beilstein Journal of Nanotechnology 2023, 14, 725–737
DOI: https://doi.org/10.3762/bjnano.14.59

The article “Cross-sectional Kelvin probe force microscopy on III–V epitaxial multilayer stacks: challenges and perspectives” by Mattia da Lisca, José Alvarez, James P. Connolly, Nicolas Vaissiere, Karim Mekhazni, Jean Decobert and Jean-Paul Kleider is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. The images or other third-party material in this article are included in the article’s Creative Commons license, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons license and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this license, visit https://creativecommons.org/licenses/by/4.0/.

Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy

Nano-piezoelectric materials such as 1D piezoelectric nanofibers, nanowires, and nanobelts have attracted a lot of research interest in recent years. *

Because of their active property that can transform strain energy into electricity, 1D piezoelectric nano-materials can be building blocks for nano-generators, strain sensors, acoustic sensors, force sensors, biosensors, self-powered drug delivery systems, piezoelectric transistors and other intelligent systems. *

The most important property of these active materials is their ability to convert mechanical energy into electrical energy and vice versa. *

Therefore, researchers started developing nano-sized piezoelectric materials in hope of achieving better piezoelectric properties. *

The characterization of these piezoelectric properties, especially measuring the piezoelectric strain coefficients, remains a challenge. *

The Atomic Force Microscopy (AFM)-based method to directly measure nano-materials’ piezoelectric strain coefficients is widely used.

However, several factors such as the extremely small piezoelectric deformation, the influence from the parasitic electrostatic force, and the environmental noise can make the measurement results questionable. *

In the article “Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy” Guitao Zhang, Xi Chen, Weihe Xu, Wei-Dong Yao, and Yong Shi address these issues by introducing a resonant piezo-force microscopy method and describing how it was used to accurately measure the piezoelectric deformation from 1D piezoelectric nanofibers. *

During the measurement the AFM tip was brought into contact with the piezoelectric sample and set to work close to the AFM tip’s first resonant frequency. *

The AFM probe used in this test was a platinum iridium coated NanoWorld Arrow-CONTPt (typical force constant 0.2 N/m, typical resonant frequency 14 KHz. The PtIr coating makes the AFM tip conductive and at the same time enhances the laser reflection from the detector facing side of the AFM cantilever to the photodetector. *

A lock-in amplifier was used to pick up the sample’s deformation signal at the testing frequency. By using this technique, the piezoelectric strain constant d33 of the Lead Zirconate Titanate (PZT) nanofiber with a diameter of 76 nm was measured. The result showed that d33 of this PZT nanofiber was around 387 pm/V. Meanwhile, by tracking the piezoelectric deformation phase image, domain structures inside PZT nanofibers were identified. *

Figure 5 from “Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy” by Guitao Zhang et al. : Piezoelectric deformation amplitude image from a PZT nanofiber on a silicon dioxide substrate (a) and its cross-sectional view along the horizontal direction (b). Conductive NanoWorld Arrow-CONTPt AFM probes were used for the resonant piezo-force microscopy — Figure 5 from “Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy” by Guitao Zhang et al. :
Piezoelectric deformation amplitude image from a PZT nanofiber on a silicon dioxide substrate (a) and its cross-sectional view along the horizontal direction (b).

Figure 6 from “Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy” by Guitao Zhang et al. : (a) Piezoelectric deformation phase image from a PZT nanofiber on the silicon dioxide substrate and its 3D image (b). NanoWorld Arrow-CONTPt platinum iridium 5 coated AFM probes were used. — Figure 6 from “Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy” by Guitao Zhang et al. :
(a) Piezoelectric deformation phase image from a PZT nanofiber on the silicon dioxide substrate and its 3D image (b).

*Guitao Zhang, Xi Chen, Weihe Xu, Wei-Dong Yao and Yong Shi
Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy
AIP Advances 12, 035203 (2022)
DOI: https://doi.org/10.1063/5.0081109

The article “Piezoelectric property of PZT nanofibers characterized by resonant piezo-force microscopy” by Guitao Zhang, Xi Chen, Weihe Xu, Wei-Dong Yao and Yong Shi is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons license, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons license and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this license, visit https://creativecommons.org/licenses/by/4.0/.

Impact of annealing on electric and elastic properties of 10-nm Hf0.5Zr0.5O2 films prepared on Si by sputtering

HfO2-based films are important materials used in broad range of electronic applications from high-performance transistors and memory cells, to thermoelectric and energy harvesting elements. *

In the article “Impact of annealing on electric and elastic properties of 10-nm Hf0.5Zr0.5O2 films prepared on Si by sputtering” Leonid Bolotov, Shinji Migita, Ryouta Fujio, Manabu Ishimaru, Shogo Hatayama and Noriyuki Uchida described how they used scanning probe methods to make nanoscale comparison of chemical composition, surface morphology, the elastic modulus and the surface potential of bare 10-nm thick Hf0.5Zr0.5O2 films prepared on Si by a carbon-free sputtering process. *

NanoWorld conductive platinum iridium5 coated Pointprobe® EFM AFM probes were used for the electrostatic force microscopy (EFM). *

The composition mapping confirmed uniform distribution of Hf and Zr in the film along wafer size. Suppression of the monoclinic phase in films annealed at 600 – 800 °C had strong impact on spatial variations of film properties. Small surface roughness, large electric domain sizes (50–200 nm at 700 °C) and small fluctuations of the surface potential (40–50 meV) in Si coated with the films are appealing for gate-stack applications. Films annealed at 600-700 °C showed the elastic modulus of about 169 GPa and the ferroelectric polarization reversal at a field of ~1 MV/cm as observed by nanoscale poling with a Pt-coated scanning probe. In contrast, properties of films annealing at 800 °C were affected by growth of thick interfacial oxide layer. *

The nanoscale approach presented in the article is beneficial in optimizing of physical and mechanical properties of thin dielectric films. *

Fig. 3 from Leonid Bolotov et al. “Impact of annealing on electric and elastic properties of 10-nm Hf0.5Zr0.5O2 films prepared on Si by sputtering”: AFM topographs (a, c) and CPD maps (b, d) of 10 nm Hf0.5Zr0.5O2 films on Si: as-grown film (a, b), and annealed at 700 °C (c, d). Rectangular shapes in (c, d) outline one domain. Scale bars are 200 nm. NanoWorld conductive platinum iridium5 coated Pointprobe® EFM AFM probes were used for the electrostatic force microscopy (EFM). — Fig. 3 from Leonid Bolotov et al. “Impact of annealing on electric and elastic properties of 10-nm Hf0.5Zr0.5O2 films prepared on Si by sputtering”:
AFM topographs (a, c) and CPD maps (b, d) of 10 nm Hf0.5Zr0.5O2 films on Si: as-grown film (a, b), and annealed at 700 °C (c, d). Rectangular shapes in (c, d) outline one domain. Scale bars are 200 nm.

*Leonid Bolotov, Shinji Migita, Ryouta Fujio, Manabu Ishimaru, Shogo Hatayama and Noriyuki Uchida
Impact of annealing on electric and elastic properties of 10-nm Hf0.5Zr0.5O2 films prepared on Si by sputtering
Microelectronic Engineering, Volume 258, 1 April 2022, 111770
DOI: https://doi.org/10.1016/j.mee.2022.111770

Open Access The article “Impact of annealing on electric and elastic properties of 10-nm Hf0.5Zr0.5O2 films prepared on Si by sputtering” by Leonid Bolotov, Shinji Migita, Ryouta Fujio, Manabu Ishimaru, Shogo Hatayama and Noriyuki Uchida is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons license, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons license and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this license, visit http://creativecommons.org/licenses/by/4.0/.