Applications of analytical electron microscopy to guide the design of boron carbide

Compositional analysis of boron carbide on nanometer length scales to examine or interpret atomic mechanisms, for example, solid-state amorphization or grain-boundary segregation, is challenging. This work reviews advancements in high-resolution microanalysis to characterize multiple generations of boron carbide. First, ζ-factor microanalysis will be introduced as a powerful (scanning) transmission electron microscopy ((S)TEM) analytical framework to accurately characterize boron carbide. Three case studies involving the application of ζ-factor microanalysis will then be presented: (1) accurate stoichiometry determination of B-doped boron carbide using ζ-factor microanalysis and electron energy loss spectroscopy, (2) normalized quantification of silicon grain-boundary segregation in Si-doped boron carbide, and (3) calibration of a scanning electron microscope X-ray energy-dispersive spectroscopy (XEDS) system to measure compositional homogeneity differences of B/Si-doped arc-melted boron carbides in the as-melted and annealed conditions. Overall, the improvement and application of advanced analytical tools have helped better understand processing–microstructure–property relationships and successfully manufacture high-performance ceramics.     

日本の寒地，北海道における2030年代の水稲生育への温暖化の影響予測とその対応(日语原文)

北海道では1980年代から2010年代まで，水稲圃場栽培期間である5–9月の気温は年代とともに上昇した。そこで，直近の2010年代（2010—2019年平均）と比べて， 2つの2030年代の予測気象から，既報の関係式より水稲生育を予測した。その結果，2030年代では2010年代に比べ，限界移植日（移植早限）が水稲栽培17地域の平均で8～9日早い。また，早限出穂期が1～5日早く，晩限出穂期が1～5日遅く，安全出穂期間が2～10日長い。出穂期は1～3日早い。出穂期から晩限出穂まで2～9日長いため，遅延型冷害の発生がやや少ない。生育期別気象は，出穂前24日以降30日間では生育が早いため平均気温が同じかやや低い。出穂前10日以降40日間および出穂期以降40日間では平均気温がやや高く，日射量はやや少ない。そのため，玄米収量は96～98％とやや低く，潜在収量性を示す気候登熟量示数は同じである。障害不稔発生に関係する穂ばらみ期冷害危険期の平均気温はわずかに低いかほぼ同じであるため，冷害発生の危険性は残る。一方，不稔発生をもたらす低温域の出現頻度には，地域間で差異がある。精米蛋白質含有率は同じであるが，アミロース含有率はやや低く，やや良食味である。米粒外観品質では被害粒歩合と着色粒歩合は一定の傾向がなく，未熟粒歩合はやや高い。精米白度は同じであるが，玄米白度はやや高い。以上の予測に対する技術的対応方向を示した。     

Methods and mechanisms for uniformly refining deformed mixed and coarse grains inside a solution-treated Ni-based superalloy by two-stage heat treatment

The uniform refinement mechanisms and methods of deformed mixed and coarse grains inside a solution-treatment Ni-based superalloy during two-stage annealing treatment have been investigated.The two-stage heat treatment experiments include an aging annealing treatment(AT)and a subsequent recrystallization annealing treatment(RT).The object of AT is to precipitate some δ phases and consume part of storage energy to inhibit the grain growth during RT,while the RT is to refine mixed and coarse grains by recrystallization.It can be found that the recrystallization grains will quickly grow up to a large size when the AT time is too low or the RT temperature is too high,while the deformed coarse grains cannot be eliminated when the AT time is too long or the RT temperature is too low.In addition,the mixed microstructure composed of some abnormal coarse recrystallization grains(ACRGs)and a large number of fine grains can be observed in the annealed specimen when the AT time is 3 h and RT tem-perature is 980℃.The phenomenon attributes to the uneven distribution of δ phase resulted from the heterogeneous deformation energy when the AT time is too short.In the regions with a large number of δ phases,the recrystallization nucleation rate is promoted and the growth of grains is limited,which results in fine grains.However,in the regions with few δ phases,the recrystallization grains around grain boundaries can easily grow up,and the new recrystallization nucleus is difficult to form inside grain,which leads to ACRGs.Thus,in order to obtain uniform and fine annealed microstructure,it is a prereq-uisite to precipitate even-distributed δ phase by choosing a suitable AT time,such as 12 h.Moreover,a relative high RT temperature is also needed to promote the recrystallization nucleation around δ phase.The optimal annealing parameters range for uniformly refining mixed crystal can be summarized as:900℃×12 h+990℃×(40-60 min)and 900℃×12 h+1000℃×(10-15 min).     

Highly oriented α-Al2O3 transparent ceramics shaped by shear force

Alumina platelets were arranged horizontally in submicron alumina particles by shear force in the flow of slurries during casting. The obtained alumina green bodies with platelets were pressureless-sintered in vacuum, producing ceramics with thoroughly oriented grains and high transmittance. The effects of sintering parameters on the densification, microstructure evolution, and orientation degree of alumina ceramics were investigated and discussed. The results showed that the densification, grain size, orientation degree, and in-line transmittance were increased with increasing sintering temperature. The enhancement of orientation degree was mainly coherent with grain growth. The grain-oriented samples exhibited a much higher in-line transmittance (at 600 nm) of 61 % than that of the grain random sample (29 %). Moreover, the transmission remained a high level in the ultraviolet range (<300 nm).     

Direct writing of textured ceramics using anisotropic nozzles

Direct writing is a unique means to align anisotropic particles for the fabrication of textured ceramics by templated grain growth (TGG). We show that alignment of tabular barium titanate (BT) template particles (20–40 μm width and 0.5–2 μm thickness) in a PIN-PMN-PT matrix powder (d₅₀ = 280 nm) is significantly improved during direct writing using anisotropic nozzles at high printing rates. The particle orientation distribution in as-printed filaments, and the texture orientation distribution in sintered ceramic filaments are shown to directly correlate with COMSOL Multiphysics-predicted torque distributions for direct writing with aspect ratio 2, 3 and 5 oval nozzles. Electromechanical strain properties of the textured piezoelectric ceramics significantly improved relative to random ceramics when printed with anisotropic nozzles. Simulations of aspect ratio 20 nozzles and nozzles with interior baffles demonstrate significantly increased torque and near elimination of constant shear stress cores (i.e. plug flow).     

Inter-Sample and Intra-Sample Variability in Electronic Properties of Methylammonium Lead Iodide

While the challenges associated with the stability of metal halide perovskites are well known and intensely studied, variability in electronic properties represents an equally significant, yet seldom studied, challenge that could potentially slow or inhibit the commercial viability of these systems. In this work, the contactless characterization technique time-resolved microwave conductivity (TRMC) is used to quantify the variability in electronic properties of the prototypical perovskite, methylammonium lead iodide (MAPbI₃) both between different samples, and at different locations within the same sample. Using scanning electron microscopy (SEM) and a quasi-automated image-analysis strategy, it is possible to evaluate the metrics of heterogeneity in surface microstructure and correlate them with the electronic properties as obtained by TRMC. Substantial intra-sample and inter-sample variation is observed in the mobility-yield product in samples prepared following differing protocols, and in samples prepared following identical protocols.     

Altered age-hardening behavior in the ultrafine-grained surface layer of Mg-Zn-Y-Ce-Zr alloy processed by sliding friction treatment

To gain insight into the ageing behavior of ultrafine grain(UFG)structure,the precipitation phenom-ena and microstructural evolutions of Mg-6Zn-1Y-0.4Ce-0.5 Zr(wt.％)alloy processed by sliding friction treatment(SFT)were systematically studied using hardness texting,transmission electron microscopy(TEM)equipped with high-angle annular dark-field scanning(HADDF-STEM),X-ray diffraction(XRD)and XRD line broadening analysis.The microhardness of the SFT-processed(SFTed)sample initially decreases from 109.6 HV to 104.8 HV at ageing for 8 h,and then increases to the peak-ageing point of 115.4 HV at 16 h.Subsequently,it enters the over-aged period.The un-SFTed sample,as the counterpart,follows a regular ageing behavior that increases from 89.9 HV to 99.6 HV when ageing for 12 h,and then drops.A multi-mechanistic model is established to describe the strengthening due to grain refinement,disloca-tion accumulation,precipitation etc.The analysis reveals that the temperature sensitive UFG structure has an obvious grain coarsening effect,which arouses the soft phenomenon in the early ageing stage.But precipitation hardening provides an excellent hardness enhancement for overcoming the negative influ-ence and helping to reach the peak-aged point.In our microstructural observations,a lot of equilibrium ultrafine MgZn2 precipitates precipitate along dislocations because defects can provide the favorable conditions for the migration and segregation of solute atoms.     

Digital twin-based analysis of volumetric error mapping procedures

The evaluation of the volumetric accuracy of a machine tool is an open challenge in the industry, and a wide variety of technical solutions are available in the market and at research level. All solutions have advantages and disadvantages concerning which errors can be measured, the achievable uncertainty, the ease of implementation, possibility of machine integration and automation, the equipment cost and the machine occupation time, and it is not always straightforward which option to choose for each application. The need to ensure accuracy during the whole lifetime of the machine and the availability of monitoring systems developed following the Industry 4.0 trend are pushing the development of measurement systems that can be integrated in the machine to perform semi-automatic verification procedures that can be performed frequently by the machine user to monitor the condition of the machine. Calibrated artefact based calibration and verification solutions have an advantage in this field over laser based solutions in terms of cost and feasibility of machine integration, but they need to be optimized for each machine and customer requirements to achieve the required calibration uncertainty and minimize machine occupation time.This paper introduces a digital twin-based methodology to simulate all relevant effects in an artefact-based machine tool calibration procedure, from the machine itself with its expected error ranges, to the artefact geometry and uncertainty, artefact positions in the workspace, probe uncertainty, compensation model, etc. By parameterizing all relevant variables in the design of the calibration procedure, this simulation methodology can be used to analyse the effect of each design variable on the error mapping uncertainty, which is of great help in adapting the procedure to each specific machine and user requirements. The simulation methodology and the analysis possibilities are illustrated by applying it on a 3-axis milling machine tool.