Ferroelectric polymer nanocomposites possess exceptional electric properties with respect to the two otherwise uniform phases,which is commonly attributed to the critical role of the matrix-particle interfacial region...Ferroelectric polymer nanocomposites possess exceptional electric properties with respect to the two otherwise uniform phases,which is commonly attributed to the critical role of the matrix-particle interfacial region.However,the structure-property correlation of the interface remains unestablished,and thus,the design of ferroelectric polymer nanocompos-ite has largely relied on the trial-and-error method.Here,a strategy that combines multi-mode scanning probe microscopy-based electrical charac-terization and nano-infrared spectroscopy is developed to unveil the local structure-property correlation of the interface in ferroelectric polymer nano-composites.The results show that the type of surface modifiers decorated on the nanoparticles can significantly influence the local polar-phase content and the piezoelectric effect of the polymer matrix surrounding the nano-particles.The strongly coupled polar-phase content and piezoelectric effect measured directly in the interfacial region as well as the computed bonding energy suggest that the property enhancement originates from the formation of hydrogen bond between the surface modifiers and the ferroelectric polymer.It is also directly detected that the local domain size of the ferroelectric polymer can impact the energy level and distribution of charge traps in the interfacial region and eventually influence the local dielectric strength.展开更多
The elastic indentation modulus and hardness of standard bulk materials and advanced thin films were determined by using the nanoindentation technique followed by the Oliver- Pharr post-treatment. After measurements w...The elastic indentation modulus and hardness of standard bulk materials and advanced thin films were determined by using the nanoindentation technique followed by the Oliver- Pharr post-treatment. After measurements with different loading/unloading schemes on chemically polished bulk titanium a substantial decrease of both modulus and hardness vs an increasing loading time was found. Then, hard nanostructured TiBN and TiCrBN thin films deposited by magnetron sputtering （using multiphase targets） on substrates of high roughness （sintered hard metal） and low roughness （silicon） were studied. Experimental modulus and hardness characterized by using two different nanoindenter tools were within the limits of standard deviation. However, a strong effect of roughness on the spread of the experimental values was observed and it was found that hardness and elastic indentation modulus obeyed a Gaussian distribution. The experimental data were discussed together with scanning probe microscopy （SPM） images of typical imprints taken after the nanoindentation tests and the local topographyls strong correlation with the results of nanoindentation was described.展开更多
The microscopic physical properties of Hardened Cement Paste (HCP) surfaces were evaluated by using Scanning Probe Microscopy (SPM). The cement pastes were cured under a hydrostatic pressure of 400 MPa and the contact...The microscopic physical properties of Hardened Cement Paste (HCP) surfaces were evaluated by using Scanning Probe Microscopy (SPM). The cement pastes were cured under a hydrostatic pressure of 400 MPa and the contacting surfaces with a slide glass during the curing were studied. Scanning Electron Microscope (SEM) observation at a magnification of 7000 revealed smooth surfaces with no holes. The surface roughness calculated from the SPM measurement was 4 nm. The surface potential and the frictional force measured by SPM were uniform throughout the measured area 24 h after the curing. However, spots of low surface potential and stains of low frictional force and low viscoelasticity were observed one month after curing. This change was attributed to the carbonation of hydrates.展开更多
One of the most intriguing methods of mitigating the hydrogen embrittlement of steels entails nano-precipitates that can trap H from enriching at vulnerable locations.However,controversial findings have been reported ...One of the most intriguing methods of mitigating the hydrogen embrittlement of steels entails nano-precipitates that can trap H from enriching at vulnerable locations.However,controversial findings have been reported on whether the incoherent NbC precipitates trap hydrogen.Here,by using in-situ scan-ning Kelvin probe force microscopy(SKPFM),we reveal the dynamic interaction of H with the border area of incoherent NbC nanoprecipitates in steel.Results indicate that the interaction between H flux and the interfaces varies amongst different precipitates,implying that H-trapping behaviours of incoherent NbC precipitates could be intrinsically diverse.Potential origins underlying the distinct behaviours are analyzed.展开更多
In this work,we investigate cross-sectional sample preparation for atomic force microscopy and general scanning probe microscopy(SPM)characterization.In light of traditional cross-sectional sample preparation solution...In this work,we investigate cross-sectional sample preparation for atomic force microscopy and general scanning probe microscopy(SPM)characterization.In light of traditional cross-sectional sample preparation solutions for transmission electron microscopy,mechanical polishing and focused ion beam(FIB)milling have been employed to prepare cross-sectional samples for SPM.We present an optimized solution for thin films and oxide heterostructures that allows for examining the prepared surfaces using various SPM techniques.In particular,post-cleaning after FIB milling is shown to be crucial and precision ion polishing was conducted to remove rough layers on mechanically polished samples.We also study SPM mechanical milling to remove amorphous layers on FIB-milled samples.Consequently,a reliable solution for making cross sections suitable for SPM has been achieved providing a useful methodology that can also be employed for other material systems with different hardness,such as polymers and metals.展开更多
Carbon,as an indispensable chemical element on Earth,has diverse covalent bonding ability,which enables construction of extensive pivotal carbon-based structures in multiple scientific fields.The extraordinary physico...Carbon,as an indispensable chemical element on Earth,has diverse covalent bonding ability,which enables construction of extensive pivotal carbon-based structures in multiple scientific fields.The extraordinary physicochemical properties presented by pioneering synthetic carbon allotropes,typically including fullerenes,carbon nanotubes,and graphene,have stimulated broad interest in fabrication of carbon-based nanostructures and nanomaterials.Accurate regulation of topology,size,and shape,as well as controllably embedding target sp^(n)-hybridized carbons in molecular skeletons,is significant for tailoring their structures and consequent properties and requires atomic precision in their preparation.Scanning probe microscopy(SPM),combined with on-surface synthesis strategy,has demonstrated its capabilities in fabrication of various carbon-based nanostructures and nanomaterials with atomic precision,which has long been elusive for conventional solution-phase synthesis due to realistic obstacles in solubility,isolation,purification,etc.More intriguingly,atom manipulation via an SPM tip allows unique access to local production of highly reactive carbon-based nanostructures.In addition,SPM provides topographic information of carbon-based nanostructures as well as their characteristic electronic structures with unprecedented submolecular resolution in real space.In this review,we overview recent exciting progress in the delicate application of SPM in probing low-dimensional carbon-based nanostructures and nanomaterials,which will open an avenue for the exploration and development of elusive and undiscovered carbon-based nanomaterials.展开更多
Scanning probe microscopes (SPM) are limited in their speed of data acquisition by the mechanical stability of the scanner. Therefore many types of scanners have been developed to achieve a rigid setup while maintaini...Scanning probe microscopes (SPM) are limited in their speed of data acquisition by the mechanical stability of the scanner. Therefore many types of scanners have been developed to achieve a rigid setup while maintaining an acceptable image size. We have followed here a different path to accelerate data acquisition by improving the feedback loop to achieve the same SPM image quality in a shorter time. While the feedback loop in a scanning probe microscope typically starts to probe a new pixel starting from the previous position, we have reduced the total control time by using an improved starting point for the feedback loop at each pixel. By exploiting the information of the already scanned pixels a forecast for the new pixel is created. We have successfully used several simple methods for a prognosis in MATLAB simulations like one dimensional linear or cubic extrapolation and others. Only scanning tunnelling microscope data from real experiments were used to test the forecasts. A doubling of the speed was achieved in the most favourable cases.展开更多
Energy storage property of a dielectric is closely tied with its nanostructure.In this study,we aim to achieve a deep understanding of this relationship in high energy density ferroelectric ceramicfilms,by probing int...Energy storage property of a dielectric is closely tied with its nanostructure.In this study,we aim to achieve a deep understanding of this relationship in high energy density ferroelectric ceramicfilms,by probing into the nanograin and sub-grain nanostructures in polycrystalline BaTiO_(3)films integrated on Si.Through scanning probe acoustic microscopy analyses,it is revealed that the BaTiO_(3)films directly grown on Pt/Ti/Si mostly consist of large discontinuous columnar nanograins,while those grown on LaNiO_(3)-buffered Pt/Ti/Si substrates have a dominant microstructure of continuous columnar nanograins.Furthermore,ultrafine ferroelastic domains of~10 nm wide are revealed inside the grains of the buffered BaTiO_(3)films,while those unbufferedfilms show about~50%increase in the domain width.The dielectric properties of the BaTiO_(3)films are well correlated with their characteristic nanostructures.Under an increasing electricfield,the LaNiO_(3)-bufferedfilms display a slower decline in its dielectric constant and a later saturation of its electric polarization,leading to an improved energy storage performance.Devicelevel charge-discharge tests have verified not only the delayed polarization saturation and high energy density of the LaNiO_(3)-buffered BaTiO_(3)film capacitors,but also a high power density in the same order as those of the ferroelectric ceramics.展开更多
Ultrafast electron sources, which enable high spatiotemporal resolution in time-resolved electron microscopy and scanning probe microscopy, are receiving increased attention. The most widely used method for achieving ...Ultrafast electron sources, which enable high spatiotemporal resolution in time-resolved electron microscopy and scanning probe microscopy, are receiving increased attention. The most widely used method for achieving ultrafast electron sources involves irradiating metal tips by ultrashort laser pulses, causing electron beam emission via the photoelectric effect [including photon-driven(quantum) or field-driven(classical) emission]. However, the thermionic electrons emission process due to the heating effect of ultrashort lasers, particularly its dynamic aspects, has rarely been addressed in previous studies. In this paper, we improved the signal-to-noise ratio of a two-pulse correlation measurement on the tip electron emission by nearly two orders of magnitude using a delay time modulation method. This allowed us to obtain information on the temperature evolution of hot electrons and phonons in a non-equilibrium state, and to extract characteristic time scales for electron-phonon and phonon-phonon scattering. Our findings indicate that the thermionic electrons emission, unlike the instantaneous photoelectric effect, causes electron emission to lag behind the laser pulse by tens of picoseconds, thus significantly affecting the detection of ultrafast dynamics of samples. Furthermore, such a lagging effect was found to be sensitive to the local structure of the metal tip, offering new insights into the improved design of ultrafast electron sources.展开更多
Surface with well-defined components and structures possesses unique electronic,magnetic,optical and chemical properties.As a result,surface chemistry research plays a crucial role in various fields such as catalysis,...Surface with well-defined components and structures possesses unique electronic,magnetic,optical and chemical properties.As a result,surface chemistry research plays a crucial role in various fields such as catalysis,energy,materials,quantum,and microelectronics.Surface science mainly investigates the correspondence between surface property and functionality.Scanning probe microscopy(SPM)techniques are important tools to characterize surface properties because of the capability of atomic-scale imaging,spectroscopy and manipulation at the single-atom level.In this review,we summarize recent advances in surface electronic,magnetic and optical properties characterized mainly by SPM-based methods.We focus on elucidating theπ-magnetism in graphene-based nanostructures,construction of spin qubits on surfaces,topology properties of surface organic structures,STM-based light emission,tip-enhanced Raman spectroscopy and integration of machine learning in SPM studies.展开更多
On-surface Ullmann-type reaction,or the dehalogenated coupling,is arguably the most pivotal reaction in on-surface synthesis for the fabrications of carbon nanostructures.Hitherto,the vast majority of works rely on ac...On-surface Ullmann-type reaction,or the dehalogenated coupling,is arguably the most pivotal reaction in on-surface synthesis for the fabrications of carbon nanostructures.Hitherto,the vast majority of works rely on activating the C-Br bond of aryl bromide which has a moderate bond dissociation energy.The C-Cl bond of aryl chloride has a higher dissociation energy and requires much higher thermal energy to break the bond.In this study,we have explored the on-surface photo-induced dechlorination and achieved the activation of three distinct aryl chlorines on the Au(111)surface with mild temperatures.This work enriches our understanding of on-surface photo-induced reactions and highlights the potential of photochemistry in realizing unconventional reactions.展开更多
Adding Ti particles to magnesium alloy simultaneously enhances its strength and ductility.However,how these particles influence on Mg alloy’s corrosion performance is seldom reported.The corrosion behavior of AZ31-Ti...Adding Ti particles to magnesium alloy simultaneously enhances its strength and ductility.However,how these particles influence on Mg alloy’s corrosion performance is seldom reported.The corrosion behavior of AZ31-Ti composites containing titanium nanoparticles(1.5 and 5 wt%)and micron particles(10 wt%)prepared by powder metallurgical in 3.5 wt%NaCl solution was investigated.The results indicate that Ti particles serve as the primary location for the cathodic hydrogen reduction reaction,resulting in intense galvanic corrosion between the Ti and Mg matrix.Ti nanoparticles distributed at the interface of the original AZ31 powder were in a discontinuous mesh structure,thus failing to act as a barrier against corrosion.The corrosion products with the existence of numerous cracks gradually peel off during the corrosion process and cannot protect the matrix.The average corrosion rate P_(w) of AZ31,AZ31-1.5%Ti,AZ31-5%Ti,and AZ31-10%Ti after 7 days of immersion is 27.55,105.65,283.67,and 99.35 mm/y,respectively.Therefore,AZ31-Ti composites can be considered as potential candidates for degradable fracturing tools.Otherwise,it is recommended to improve their corrosion resistance through surface treatment.展开更多
The phosphate protective film and micro-galvanic corrosion of biological Mg-3Zn-xNd (x = 0, 0.6, 1.2) alloys were investigated by scanning and transmission electron microscopy, quasi-in-situ observation, scanning Kelv...The phosphate protective film and micro-galvanic corrosion of biological Mg-3Zn-xNd (x = 0, 0.6, 1.2) alloys were investigated by scanning and transmission electron microscopy, quasi-in-situ observation, scanning Kelvin probe force microscopy (SKPFM) and electrochemical tests. The results revealed the Mg-Zn-Nd phases formed in Mg-3Zn alloy contained with Nd. Adding Nd resulted in a significant decline in the cracks of the phosphate protective film and micro-galvanic corrosion of alloys, which were recorded by quasi-in-situ observation. In addition, the Volta potential difference of Mg-Zn-Nd/α-Mg (~ 188 mV) was lower than MgZn/α-Mg (~ 419 mV) and Zn-rich/α-Mg (~ 260 mV), and the corrosion rates of alloys markedly decreased after the addition of 0.6 wt% Nd. The improvement in corrosion resistance of Nd-containing alloys was mainly attributed to the following: (i) the addition of Nd reduced the Volta potential difference (second phases/α-Mg);(ii) the phosphate protective film containing Nd_(2)O_(3) deposited on the surface of the alloys, effectively preventing the penetration of harmful anions.展开更多
The work combined scanning Kelvin probe force microscopy measurements and finite element modelling to study the diffusion and distribution of hydrogen(H)atoms at metallurgical microphases contained in X52 pipeline ste...The work combined scanning Kelvin probe force microscopy measurements and finite element modelling to study the diffusion and distribution of hydrogen(H)atoms at metallurgical microphases contained in X52 pipeline steel.Results show that the pearlite contained in the steel is more stable than the ferrite during electropolishing,as indicated by the measured topographic profiles and Volta potentials.The hydrogen(H)-charging enhances the electrochemical activity of both pearlite and ferrite,as shown by increased Volta potential and thus the decreased work function.As the H-charging time increases,the Volta potentials of both phases further increase,implying that their activities increase with the H-charging time.The pearlite has a greater Volta potential and thus a lower work function than the ferrite.This is associated with more H atoms accumulating at the pearlite than at the ferrite.The H atom diffusion and accumulation are affected by H diffusivity at phase boundaries,H-trap binding energy and the number of traps in the steel.展开更多
During heat treatment processing, microstructures of heat affected zone （HAZ） were formed in X80 pipe- line steel. After observation by optical microscopy, scanning electron microscopy and transmission electron micr...During heat treatment processing, microstructures of heat affected zone （HAZ） were formed in X80 pipe- line steel. After observation by optical microscopy, scanning electron microscopy and transmission electron microsco- py, microstructure of the as-received X80 steel was confirmed to be acicular ferrite, while the microstructures of quenched, normalized and annealed X80 steels were lath bainite, granular ferrite and quasi-polygonal ferrite, respec- tively. After immersion in the simulated acidic soil solution for 48 h, corrosion rates of these four steels were deter- mined by mass loss measurements and corrosion products were examined by Raman spectroscopy and X-ray photoe lectron spectroscopy. Scanning vibrating electrode technique was used to characterize the micro-galvanic corrosion be- haviors of the synthetic bimetallic electrodes which were formed by coupling each of the simulated HAZ microstruc- tures with the as-received steel in direct physical and electric contact. It is demonstrated that the as-received steel acts as cathode in the as-received/quenched and as-received/normalized couples, while the annealed steel acts as cathode when coupling with the as received steel. The distinction of current density between the galvanic couples reduces with prolonging the immersion time.展开更多
We succeeded in performing of hybrid Scanning Probe Microscopy (hybrid-SPM) in which mechanical-SPM andfluorescence microscopy are combined. This technique is able to measure simultaneously mechanical properties anddi...We succeeded in performing of hybrid Scanning Probe Microscopy (hybrid-SPM) in which mechanical-SPM andfluorescence microscopy are combined. This technique is able to measure simultaneously mechanical properties anddistribution of cytoskeletons of living cells by using green fluorescent protein. We measured evolution of both local elasticityand distributions of actin stress fibers in an identical fibroblast living in physiological conditions. The SPM experimentsrevealed that stiffer lines develop in living cells, which correspond to actin stress fibers. The elasticity of the actin stressfibers is as high as 100 kPa. We discuss mechanical effects on the development of actin filament networks.展开更多
A highly distorted chiral nanographene structure composed of triple corannulene-fused[5]helicenes is prepared with the help of the Heck reaction and oxidative photocyclization with an overall isolated yield of 28%.The...A highly distorted chiral nanographene structure composed of triple corannulene-fused[5]helicenes is prepared with the help of the Heck reaction and oxidative photocyclization with an overall isolated yield of 28%.The complex three-dimensional(3D)structure of the bowl-helix hybrid nanostructure is studied by a combination of noncontact atomic force microscopy(AFM)and scanning tunneling microscopy(STM)on the Cu(111)surface,density functional theory calculations,AFM/STM simulations,and high-performance liquid chromatography-electronic circular dichroism analysis.This examination reveals a molecular structure in which the three bowl-shaped corannulene bladesd position themselves in a C3-symmetric fashion around a highly twisted triphenylene core.The molecule appears to be shaped like a propeller in which the concave side of the bowls face away from the connected[5]helicene motif.The chirality of the nanostructure is confirmed by the direct visualization of both MMM and PPP enantiomers at the single-molecule level by scanning probe microscopies.These results underline that submolecular resolution imaging by AFM/STM is a powerful real-space tool for the stereochemical characterization of 3D curved chiral nanographene structures.展开更多
By employing scanning probe microscopy,conductive path and local oxygen-vacancy dynamics have been investigated in crosshatched La_(0.7)Sr_(0.3)MnO_(3) thin films grown onto flat and vicinal LaAlO_(3)(001)single cryst...By employing scanning probe microscopy,conductive path and local oxygen-vacancy dynamics have been investigated in crosshatched La_(0.7)Sr_(0.3)MnO_(3) thin films grown onto flat and vicinal LaAlO_(3)(001)single crystal substrates.Consistent with prior studies,the crosshatch topography was observed first by dynamical force microscopy as the epi-stain started to release with increasing film thickness.Second,by using conductive atomic force microscopy(CAFM),conductive crosshatch and dots(locally aligned or random)were unravelled,however,not all of which necessarily coincided with that shown in the in situ atomic force microscopy.Furthermore,the current-voltage responses were probed by CAFM,revealing the occurrence of threshold and/or memristive switchings.Our results demonstrate that the resistive switching relies on the evolution of the local profile and concentration of oxygen vacancies,which,in the crosshatched films,are modulated by both the misfit and threading dislocations.展开更多
Duplex stainless steels(DSSs)are suffering from various localized corrosion attacks such as pitting,selective dissolution,crevice corrosion during their service period.It is of great value to quantitatively analyze an...Duplex stainless steels(DSSs)are suffering from various localized corrosion attacks such as pitting,selective dissolution,crevice corrosion during their service period.It is of great value to quantitatively analyze and grasp the micro-electrochemical corrosion behavior and related mechanism for DSSs on the micrometer or even smaller scales.In this work,scanning Kelvin probe force microscopy(SKPFM)and energy dispersive spectroscopy(EDS)measurements were performed to reveal the difference between the austenite phase and ferrite phase in microregion of DSS 2205.Then traditional electrochemical impedance spectroscopy(EIS)and potentiodynamic polarization(PDP)tests were employed for micro-electrochemical characterization of DSS 2205 with different proportion phases inϕ40 andϕ10μm micro holes.Both of them can only be utilized for qualitative or semi-quantitative micro-electrochemical characterization of DSS 2205.Coulostatic perturbation method was employed for quantitative micro-electrochemical characterization of DSS 2205.What is more,the applicable conditions of coulostatic perturbation were analyzed in depth by establishing a detailed electrochemical interface circuit.A series of microregion coulostatic perturbations for DSS 2205 with different proportion phases inϕ10μm micro holes showed that as the austenite proportion increases,the corresponding polarization resistance of microregion increases linearly.展开更多
基金supported by the National Natural Science Foundation of China(Nos.51922056 and 51921005).
文摘Ferroelectric polymer nanocomposites possess exceptional electric properties with respect to the two otherwise uniform phases,which is commonly attributed to the critical role of the matrix-particle interfacial region.However,the structure-property correlation of the interface remains unestablished,and thus,the design of ferroelectric polymer nanocompos-ite has largely relied on the trial-and-error method.Here,a strategy that combines multi-mode scanning probe microscopy-based electrical charac-terization and nano-infrared spectroscopy is developed to unveil the local structure-property correlation of the interface in ferroelectric polymer nano-composites.The results show that the type of surface modifiers decorated on the nanoparticles can significantly influence the local polar-phase content and the piezoelectric effect of the polymer matrix surrounding the nano-particles.The strongly coupled polar-phase content and piezoelectric effect measured directly in the interfacial region as well as the computed bonding energy suggest that the property enhancement originates from the formation of hydrogen bond between the surface modifiers and the ferroelectric polymer.It is also directly detected that the local domain size of the ferroelectric polymer can impact the energy level and distribution of charge traps in the interfacial region and eventually influence the local dielectric strength.
基金supported by the "Communauté Franaise de Belgique-ARC 04/09-310"was done in the context of the EC VI FW international EXCELL Project
文摘The elastic indentation modulus and hardness of standard bulk materials and advanced thin films were determined by using the nanoindentation technique followed by the Oliver- Pharr post-treatment. After measurements with different loading/unloading schemes on chemically polished bulk titanium a substantial decrease of both modulus and hardness vs an increasing loading time was found. Then, hard nanostructured TiBN and TiCrBN thin films deposited by magnetron sputtering （using multiphase targets） on substrates of high roughness （sintered hard metal） and low roughness （silicon） were studied. Experimental modulus and hardness characterized by using two different nanoindenter tools were within the limits of standard deviation. However, a strong effect of roughness on the spread of the experimental values was observed and it was found that hardness and elastic indentation modulus obeyed a Gaussian distribution. The experimental data were discussed together with scanning probe microscopy （SPM） images of typical imprints taken after the nanoindentation tests and the local topographyls strong correlation with the results of nanoindentation was described.
文摘The microscopic physical properties of Hardened Cement Paste (HCP) surfaces were evaluated by using Scanning Probe Microscopy (SPM). The cement pastes were cured under a hydrostatic pressure of 400 MPa and the contacting surfaces with a slide glass during the curing were studied. Scanning Electron Microscope (SEM) observation at a magnification of 7000 revealed smooth surfaces with no holes. The surface roughness calculated from the SPM measurement was 4 nm. The surface potential and the frictional force measured by SPM were uniform throughout the measured area 24 h after the curing. However, spots of low surface potential and stains of low frictional force and low viscoelasticity were observed one month after curing. This change was attributed to the carbonation of hydrates.
基金supported by the National Natural Science Foun-dation of China under grant Nos.52231003,52301073,52271049,and 52201063.
文摘One of the most intriguing methods of mitigating the hydrogen embrittlement of steels entails nano-precipitates that can trap H from enriching at vulnerable locations.However,controversial findings have been reported on whether the incoherent NbC precipitates trap hydrogen.Here,by using in-situ scan-ning Kelvin probe force microscopy(SKPFM),we reveal the dynamic interaction of H with the border area of incoherent NbC nanoprecipitates in steel.Results indicate that the interaction between H flux and the interfaces varies amongst different precipitates,implying that H-trapping behaviours of incoherent NbC precipitates could be intrinsically diverse.Potential origins underlying the distinct behaviours are analyzed.
文摘In this work,we investigate cross-sectional sample preparation for atomic force microscopy and general scanning probe microscopy(SPM)characterization.In light of traditional cross-sectional sample preparation solutions for transmission electron microscopy,mechanical polishing and focused ion beam(FIB)milling have been employed to prepare cross-sectional samples for SPM.We present an optimized solution for thin films and oxide heterostructures that allows for examining the prepared surfaces using various SPM techniques.In particular,post-cleaning after FIB milling is shown to be crucial and precision ion polishing was conducted to remove rough layers on mechanically polished samples.We also study SPM mechanical milling to remove amorphous layers on FIB-milled samples.Consequently,a reliable solution for making cross sections suitable for SPM has been achieved providing a useful methodology that can also be employed for other material systems with different hardness,such as polymers and metals.
基金financial support from the National Natural Science Foundation of China(Grant Nos.22125203,21790351)the Fundamental Research Funds for the Central Universities(Grant No.22120220051).
文摘Carbon,as an indispensable chemical element on Earth,has diverse covalent bonding ability,which enables construction of extensive pivotal carbon-based structures in multiple scientific fields.The extraordinary physicochemical properties presented by pioneering synthetic carbon allotropes,typically including fullerenes,carbon nanotubes,and graphene,have stimulated broad interest in fabrication of carbon-based nanostructures and nanomaterials.Accurate regulation of topology,size,and shape,as well as controllably embedding target sp^(n)-hybridized carbons in molecular skeletons,is significant for tailoring their structures and consequent properties and requires atomic precision in their preparation.Scanning probe microscopy(SPM),combined with on-surface synthesis strategy,has demonstrated its capabilities in fabrication of various carbon-based nanostructures and nanomaterials with atomic precision,which has long been elusive for conventional solution-phase synthesis due to realistic obstacles in solubility,isolation,purification,etc.More intriguingly,atom manipulation via an SPM tip allows unique access to local production of highly reactive carbon-based nanostructures.In addition,SPM provides topographic information of carbon-based nanostructures as well as their characteristic electronic structures with unprecedented submolecular resolution in real space.In this review,we overview recent exciting progress in the delicate application of SPM in probing low-dimensional carbon-based nanostructures and nanomaterials,which will open an avenue for the exploration and development of elusive and undiscovered carbon-based nanomaterials.
文摘Scanning probe microscopes (SPM) are limited in their speed of data acquisition by the mechanical stability of the scanner. Therefore many types of scanners have been developed to achieve a rigid setup while maintaining an acceptable image size. We have followed here a different path to accelerate data acquisition by improving the feedback loop to achieve the same SPM image quality in a shorter time. While the feedback loop in a scanning probe microscope typically starts to probe a new pixel starting from the previous position, we have reduced the total control time by using an improved starting point for the feedback loop at each pixel. By exploiting the information of the already scanned pixels a forecast for the new pixel is created. We have successfully used several simple methods for a prognosis in MATLAB simulations like one dimensional linear or cubic extrapolation and others. Only scanning tunnelling microscope data from real experiments were used to test the forecasts. A doubling of the speed was achieved in the most favourable cases.
基金Natural Science Foundation of Shandong Province(Grant No.ZR2022ZD39,ZR2020QE042,ZR2022ME031,ZR2022QB138)the National Natural Science Foundation of China(NSFC)(Grant nos.51772175,52002192)+2 种基金the Science,Education and Industry Integration Pilot Projects of Qilu University of Technology(Shandong Academy of Sciences)(Grant Nos.2022GH018,2022PY055).J.Ouyang acknowledges the support from the Jinan Science and Technology Bureau(Grant No.2021GXRC055)the Education Department of Hunan Province/Xiangtan University(Grant No.KZ0807969)the seed funding for top talents at Qilu University of Technology(Shandong Academy of Sciences).
文摘Energy storage property of a dielectric is closely tied with its nanostructure.In this study,we aim to achieve a deep understanding of this relationship in high energy density ferroelectric ceramicfilms,by probing into the nanograin and sub-grain nanostructures in polycrystalline BaTiO_(3)films integrated on Si.Through scanning probe acoustic microscopy analyses,it is revealed that the BaTiO_(3)films directly grown on Pt/Ti/Si mostly consist of large discontinuous columnar nanograins,while those grown on LaNiO_(3)-buffered Pt/Ti/Si substrates have a dominant microstructure of continuous columnar nanograins.Furthermore,ultrafine ferroelastic domains of~10 nm wide are revealed inside the grains of the buffered BaTiO_(3)films,while those unbufferedfilms show about~50%increase in the domain width.The dielectric properties of the BaTiO_(3)films are well correlated with their characteristic nanostructures.Under an increasing electricfield,the LaNiO_(3)-bufferedfilms display a slower decline in its dielectric constant and a later saturation of its electric polarization,leading to an improved energy storage performance.Devicelevel charge-discharge tests have verified not only the delayed polarization saturation and high energy density of the LaNiO_(3)-buffered BaTiO_(3)film capacitors,but also a high power density in the same order as those of the ferroelectric ceramics.
基金supported by the National Key R&D Program under Grant No.2021YFA1400500the National Natural Science Foundation of China under Grant No.22273029+1 种基金the New Cornerstone Science Foundation through the New Cornerstone Investigator Program under Grant No.NCI202303 and the XPLORER PRIZEthe Beijing Outstanding Young Scientist Program under Grant No.JWZQ20240101002。
文摘Ultrafast electron sources, which enable high spatiotemporal resolution in time-resolved electron microscopy and scanning probe microscopy, are receiving increased attention. The most widely used method for achieving ultrafast electron sources involves irradiating metal tips by ultrashort laser pulses, causing electron beam emission via the photoelectric effect [including photon-driven(quantum) or field-driven(classical) emission]. However, the thermionic electrons emission process due to the heating effect of ultrashort lasers, particularly its dynamic aspects, has rarely been addressed in previous studies. In this paper, we improved the signal-to-noise ratio of a two-pulse correlation measurement on the tip electron emission by nearly two orders of magnitude using a delay time modulation method. This allowed us to obtain information on the temperature evolution of hot electrons and phonons in a non-equilibrium state, and to extract characteristic time scales for electron-phonon and phonon-phonon scattering. Our findings indicate that the thermionic electrons emission, unlike the instantaneous photoelectric effect, causes electron emission to lag behind the laser pulse by tens of picoseconds, thus significantly affecting the detection of ultrafast dynamics of samples. Furthermore, such a lagging effect was found to be sensitive to the local structure of the metal tip, offering new insights into the improved design of ultrafast electron sources.
文摘Surface with well-defined components and structures possesses unique electronic,magnetic,optical and chemical properties.As a result,surface chemistry research plays a crucial role in various fields such as catalysis,energy,materials,quantum,and microelectronics.Surface science mainly investigates the correspondence between surface property and functionality.Scanning probe microscopy(SPM)techniques are important tools to characterize surface properties because of the capability of atomic-scale imaging,spectroscopy and manipulation at the single-atom level.In this review,we summarize recent advances in surface electronic,magnetic and optical properties characterized mainly by SPM-based methods.We focus on elucidating theπ-magnetism in graphene-based nanostructures,construction of spin qubits on surfaces,topology properties of surface organic structures,STM-based light emission,tip-enhanced Raman spectroscopy and integration of machine learning in SPM studies.
基金Funding from the U.S.Army Research Laboratory under agreement No.W911NF-14–2–0005 with Dr.Joe Labukas as project manager supported co-author JMFFunding by the Office of Naval Research grant No.N000141210967 with Dr.David A.Shifler as scientific officer supported co-author LGBThe Bruker Dimension Icon AFM utilized in this work is located in the Boise State University Surface Science Laboratory(SSL),which is part of the FaCT Core Facility,RRID:SCR_024733,that receives support from the National Institutes of Health under the Institutional Development Awards Program of the National Institute of General Medical Sciences via grants#P20GM148321 and P20GM103408,the former of which also partially supports co-authors CME and PHD.
基金supported by National Natural Science Foundation of China(Nos.22072086,22302120)。
文摘On-surface Ullmann-type reaction,or the dehalogenated coupling,is arguably the most pivotal reaction in on-surface synthesis for the fabrications of carbon nanostructures.Hitherto,the vast majority of works rely on activating the C-Br bond of aryl bromide which has a moderate bond dissociation energy.The C-Cl bond of aryl chloride has a higher dissociation energy and requires much higher thermal energy to break the bond.In this study,we have explored the on-surface photo-induced dechlorination and achieved the activation of three distinct aryl chlorines on the Au(111)surface with mild temperatures.This work enriches our understanding of on-surface photo-induced reactions and highlights the potential of photochemistry in realizing unconventional reactions.
基金funded by the Guangdong Major Project of Basic and Applied Basic Research (Grant No.2020B0301030006)。
文摘Adding Ti particles to magnesium alloy simultaneously enhances its strength and ductility.However,how these particles influence on Mg alloy’s corrosion performance is seldom reported.The corrosion behavior of AZ31-Ti composites containing titanium nanoparticles(1.5 and 5 wt%)and micron particles(10 wt%)prepared by powder metallurgical in 3.5 wt%NaCl solution was investigated.The results indicate that Ti particles serve as the primary location for the cathodic hydrogen reduction reaction,resulting in intense galvanic corrosion between the Ti and Mg matrix.Ti nanoparticles distributed at the interface of the original AZ31 powder were in a discontinuous mesh structure,thus failing to act as a barrier against corrosion.The corrosion products with the existence of numerous cracks gradually peel off during the corrosion process and cannot protect the matrix.The average corrosion rate P_(w) of AZ31,AZ31-1.5%Ti,AZ31-5%Ti,and AZ31-10%Ti after 7 days of immersion is 27.55,105.65,283.67,and 99.35 mm/y,respectively.Therefore,AZ31-Ti composites can be considered as potential candidates for degradable fracturing tools.Otherwise,it is recommended to improve their corrosion resistance through surface treatment.
基金support by the National Natural Science Foundation of China(No.51961026).
文摘The phosphate protective film and micro-galvanic corrosion of biological Mg-3Zn-xNd (x = 0, 0.6, 1.2) alloys were investigated by scanning and transmission electron microscopy, quasi-in-situ observation, scanning Kelvin probe force microscopy (SKPFM) and electrochemical tests. The results revealed the Mg-Zn-Nd phases formed in Mg-3Zn alloy contained with Nd. Adding Nd resulted in a significant decline in the cracks of the phosphate protective film and micro-galvanic corrosion of alloys, which were recorded by quasi-in-situ observation. In addition, the Volta potential difference of Mg-Zn-Nd/α-Mg (~ 188 mV) was lower than MgZn/α-Mg (~ 419 mV) and Zn-rich/α-Mg (~ 260 mV), and the corrosion rates of alloys markedly decreased after the addition of 0.6 wt% Nd. The improvement in corrosion resistance of Nd-containing alloys was mainly attributed to the following: (i) the addition of Nd reduced the Volta potential difference (second phases/α-Mg);(ii) the phosphate protective film containing Nd_(2)O_(3) deposited on the surface of the alloys, effectively preventing the penetration of harmful anions.
基金supported by Mitacs,InnoTech Alberta and Natural Science and Engineering Research Council(NSERC),CanadaStudy of hydrogen atom distribution at metallurgical microphases of X52 steel by scanning Kelvin probe force microscopy and finite element modelling.
文摘The work combined scanning Kelvin probe force microscopy measurements and finite element modelling to study the diffusion and distribution of hydrogen(H)atoms at metallurgical microphases contained in X52 pipeline steel.Results show that the pearlite contained in the steel is more stable than the ferrite during electropolishing,as indicated by the measured topographic profiles and Volta potentials.The hydrogen(H)-charging enhances the electrochemical activity of both pearlite and ferrite,as shown by increased Volta potential and thus the decreased work function.As the H-charging time increases,the Volta potentials of both phases further increase,implying that their activities increase with the H-charging time.The pearlite has a greater Volta potential and thus a lower work function than the ferrite.This is associated with more H atoms accumulating at the pearlite than at the ferrite.The H atom diffusion and accumulation are affected by H diffusivity at phase boundaries,H-trap binding energy and the number of traps in the steel.
基金Sponsored by National Natural Science Foundation of China(51171025,51131001)Beijing Postdoctoral Research Foundation of China(2013M540829)
文摘During heat treatment processing, microstructures of heat affected zone （HAZ） were formed in X80 pipe- line steel. After observation by optical microscopy, scanning electron microscopy and transmission electron microsco- py, microstructure of the as-received X80 steel was confirmed to be acicular ferrite, while the microstructures of quenched, normalized and annealed X80 steels were lath bainite, granular ferrite and quasi-polygonal ferrite, respec- tively. After immersion in the simulated acidic soil solution for 48 h, corrosion rates of these four steels were deter- mined by mass loss measurements and corrosion products were examined by Raman spectroscopy and X-ray photoe lectron spectroscopy. Scanning vibrating electrode technique was used to characterize the micro-galvanic corrosion be- haviors of the synthetic bimetallic electrodes which were formed by coupling each of the simulated HAZ microstruc- tures with the as-received steel in direct physical and electric contact. It is demonstrated that the as-received steel acts as cathode in the as-received/quenched and as-received/normalized couples, while the annealed steel acts as cathode when coupling with the as received steel. The distinction of current density between the galvanic couples reduces with prolonging the immersion time.
基金This work is partially supported by the Special Funding for Basic Research, Ministry of Education, Science, Sports and Culture, Japan, to K. K.
文摘We succeeded in performing of hybrid Scanning Probe Microscopy (hybrid-SPM) in which mechanical-SPM andfluorescence microscopy are combined. This technique is able to measure simultaneously mechanical properties anddistribution of cytoskeletons of living cells by using green fluorescent protein. We measured evolution of both local elasticityand distributions of actin stress fibers in an identical fibroblast living in physiological conditions. The SPM experimentsrevealed that stiffer lines develop in living cells, which correspond to actin stress fibers. The elasticity of the actin stressfibers is as high as 100 kPa. We discuss mechanical effects on the development of actin filament networks.
基金Financial support from the Ministry of Education Singapore under the AcRF Tier 1(MOE T1 RG11/21)and AcRF Tier 2(MOE-T2EP10221-0002)The Deutsche Forschungsgemeinschaft via grants(nos.SCHI 619/13 and EB535/1-1)+5 种基金the GRK(Research Training Group)2204“Substitute Materials for Sustainable Energy Technologies”the LOEWE Program of Excellence of the Federal State of Hesse(LOEWE Focus Group PriOSS“Principles of On-Surface Synthesis”)the National Natural Science Foundation of China(grant nos.21790053,51821002,and 22072103)the National Major State Basic Research Development Program of China(grant nos.2017YFA0205000 and 2017YFA0205002)the Collaborative Innovation Center of Suzhou Nano Science&Technologythe 111 Project are also acknowledged for their financial support.
文摘A highly distorted chiral nanographene structure composed of triple corannulene-fused[5]helicenes is prepared with the help of the Heck reaction and oxidative photocyclization with an overall isolated yield of 28%.The complex three-dimensional(3D)structure of the bowl-helix hybrid nanostructure is studied by a combination of noncontact atomic force microscopy(AFM)and scanning tunneling microscopy(STM)on the Cu(111)surface,density functional theory calculations,AFM/STM simulations,and high-performance liquid chromatography-electronic circular dichroism analysis.This examination reveals a molecular structure in which the three bowl-shaped corannulene bladesd position themselves in a C3-symmetric fashion around a highly twisted triphenylene core.The molecule appears to be shaped like a propeller in which the concave side of the bowls face away from the connected[5]helicene motif.The chirality of the nanostructure is confirmed by the direct visualization of both MMM and PPP enantiomers at the single-molecule level by scanning probe microscopies.These results underline that submolecular resolution imaging by AFM/STM is a powerful real-space tool for the stereochemical characterization of 3D curved chiral nanographene structures.
基金funded by the Science Center of the National Science Foundation of China(Grant No.52088101)the National Natural Science Foundation of China(Grant Nos.11474342 and11174353)+2 种基金the National Key Research and Development Program of Chinathe Strategic Priority Research Program B of the Chinese Academy of Sciencessupported in part by the beamline 08U1A of SSRF。
文摘By employing scanning probe microscopy,conductive path and local oxygen-vacancy dynamics have been investigated in crosshatched La_(0.7)Sr_(0.3)MnO_(3) thin films grown onto flat and vicinal LaAlO_(3)(001)single crystal substrates.Consistent with prior studies,the crosshatch topography was observed first by dynamical force microscopy as the epi-stain started to release with increasing film thickness.Second,by using conductive atomic force microscopy(CAFM),conductive crosshatch and dots(locally aligned or random)were unravelled,however,not all of which necessarily coincided with that shown in the in situ atomic force microscopy.Furthermore,the current-voltage responses were probed by CAFM,revealing the occurrence of threshold and/or memristive switchings.Our results demonstrate that the resistive switching relies on the evolution of the local profile and concentration of oxygen vacancies,which,in the crosshatched films,are modulated by both the misfit and threading dislocations.
基金financial support from the Ministry of Science and Technology, China for the national key research and development plan (No. 2017YFB0701904)China Nuclear Power Engineering Co., Ltd. (No. KY1672)the 111 Project (No. B12012)
文摘Duplex stainless steels(DSSs)are suffering from various localized corrosion attacks such as pitting,selective dissolution,crevice corrosion during their service period.It is of great value to quantitatively analyze and grasp the micro-electrochemical corrosion behavior and related mechanism for DSSs on the micrometer or even smaller scales.In this work,scanning Kelvin probe force microscopy(SKPFM)and energy dispersive spectroscopy(EDS)measurements were performed to reveal the difference between the austenite phase and ferrite phase in microregion of DSS 2205.Then traditional electrochemical impedance spectroscopy(EIS)and potentiodynamic polarization(PDP)tests were employed for micro-electrochemical characterization of DSS 2205 with different proportion phases inϕ40 andϕ10μm micro holes.Both of them can only be utilized for qualitative or semi-quantitative micro-electrochemical characterization of DSS 2205.Coulostatic perturbation method was employed for quantitative micro-electrochemical characterization of DSS 2205.What is more,the applicable conditions of coulostatic perturbation were analyzed in depth by establishing a detailed electrochemical interface circuit.A series of microregion coulostatic perturbations for DSS 2205 with different proportion phases inϕ10μm micro holes showed that as the austenite proportion increases,the corresponding polarization resistance of microregion increases linearly.
