Effect of in-situ nanoparticles on the mechanical properties and hydrogen embrittlement of high-strength steel

We investigated the critical influence of in-situ nanoparticles on the mechanical properties and hydrogen embrittlement(HE)of high-strength steel.The results reveal that the mechanical strength and elongation of quenched and tempered steel(919 MPa yield strength,17.11%elongation)are greater than those of hot-rolled steel(690 MPa yield strength,16.81%elongation)due to the strengthening effect of insitu Ti_(3)O_(5)–Nb(C,N)nanoparticles.In addition,the HE susceptibility is substantially mitigated to 55.52%,approximately 30%lower than that of steels without in-situ nanoparticles(84.04%),which we attribute to the heterogeneous nucleation of the Ti_(3)O_5 nanoparticles increasing the density of the carbides.Compared with hard TiN inclusions,the spherical and soft Al_(2)O_(3)–MnS core–shell inclusions that nucleate on in-situ Al_(2)O_(3) particles could also suppress HE.In-situ nanoparticles generated by the regional trace-element supply have strong potential for the development of high-strength and hydrogen-resistant steels.

Probing the Nucleation and Growth Kinetics of Bismuth Nanoparticles via In-situ Transmission Electron Microscopy

The nucleation and growth mechanism of nanoparticles is an important theory,which can guide the preparation of nanomaterials.However,it is still lacking in direct observation on the details of the evolution of intermediate state structure during nucleation and growth.In this work,the evolution process of bismuth nanoparticles induced by electron beam was revealed by in-situ transmission electron microscopy(TEM)at atomic scale.The experimental results demonstrate that the size,stable surface and crystallographic defect have important influences on the growth of Bi nanoparticles.Two non-classical growth paths including single crystal growth and polycrystalline combined growth,as well as,corresponding layer-by-layer growth mechanism along{012}stable crystal plane of Bi nanoparticles with dodecahedron structure were revealed by in-situ TEM directly.These results provide important guidance and a new approach for in-depth understanding of the nucleation and growth kinetics of nanoparticles.

Enhanced thermal and electrical properties of poly (D,L-lactide)/ multi-walled carbon nanotubes composites by in-situ polymerization

Biodegradable poly （D,L-lactide） （PLA）/carboxyl-functionalized multi-walled carbon nanotubes （c-MWCNTs） composites were achieved via in-situ polymerization. These as-prepared composite materials were characterized with FT-IR, XRD, TG, DSC, SEM, and high insulation resistance meter. The results demonstrate that the multi-walled carbon nanotube was carboxyl functionalized, which improved the collection between c-MWCNTs and PLA, and further realized the graft copolymerization of c-MWCNTs and PLA. There is a higher glass transition temperature and a lower pyrolysis temperature of PLA/c-MWCNTs composites than pure PLA. The c-MWCNTs gave a better dispersion than unmodified MWCNTs in the PLA matrix, and an even coating of PLA on the surface of c-MWCNTs was obtained, which increased the interfacial interaction. High insulation resistance analysis showed that the addition of c-MWCNTs increased the electric conductivity, and c-MWCNTs performed against the large dielectric coefficient and electrostatic state of PLA. These results demonstrated that c-MWCNTs modified PLA composites were beneficial for potential application in the development of heat-resisting and conductivity plastic engineering.

In-situ homogeneous synthesis of carbon nanotubes on aluminum matrix and properties of their composites

Using nickel catalyst supported on aluminum powders, carbon nanotubes （CNTs） were successfully synthesized in aluminum powders by in-situ chemical vapor deposition at 650 ℃. Structural characterization revealed that the as-grown CNTs possessed higher graphitization degree and straight graphite shell. By this approach, more homogeneous dispersion of CNTs in aluminum powders was achieved compared with the traditional mechanical mixture methods. Using the in-situ synthesized CNTs/Al composite powders and powder metallurgy process, CNTs/Al bulk composites were prepared. Performance testing showed that the mechanical properties and dimensional stability of the composites were improved obviously, which was attributed to the superior dispersion of CNTs in aluminum matrix and the strong interfacial bonding between CNTs and matrix.

Mechanism and Kinetic Model of In-situ TiB_2/7055Al Nanocomposites Synthesized under High Intensity Ultrasonic Field

In-situ TiB2/7055Al nanocomposites are fabricated by in situ melt chemical reaction from 7055Al-K2TiF6-KBF4 system under high intensity ultrasonic field,and the mechanism and kinetic model of in-situ melt chemical reaction are investigated.X-ray diffraction （XRD） and scanning electron microscope （SEM） analyses indicate that the sizes of in-situ TiB2 nanoparticles are in the range of 80-120 nm.The results of ice-water quenched samples show that the whole process contains four stages,and the overall in-situ reaction time is 10 minutes.The in situ synthesis process is controlled mainly by chemical reaction in earlier stage （former 3 minutes）,and by the particulate diffusing in later stage.The mechanism of key reaction between Al3Ti and AlB2 under high intensity ultrasonic in the 7055Al-K2TiF6-KBF4 system is the reaction-diffusion-crack-rediffusion.Furthermore,the reactive kinetic models in 7055Al-K2TiF6-KBF4 system are established.

Efficient grain refinement of Al alloys induced by in-situ nanoparticles

Grain refinement of Al and Al alloys during the solidification remains a long-term challenge.Here we report a general strategy for efficient grain refinement through instantaneously in-situ forming abundant nanoparticles with concentrated size distribution.The Al-Zn-Mg-Cu alloy and commercial purity Al are respectively refined by using this proposed strategy and the traditional refinement method(adding AlTi-B alloy into Al melt),and the experimental and numerical results indicate that the TiBnanoparticles instantaneously form in the Al melt during the in-situ refinement process.Compared to the traditional refinement treatment method,the new approach not only can promote the high number density of the nucleation sites and narrow their size distribution,but also tremendously attenuates the agglomeration and settlement of the heterogeneous nucleation sites.It exhibits much better grain refinement ability and inhibits the decline of the grain refinement efficiency.This approach may have broad application prospect not only for the grain refinement of Al and Al alloys,but also for the grain refinement of other alloy systems,e.g.steel,magnesium,copper,and so on.

IN-SITU POLYMERIZED SYNTHESIS AND PROPERTIES OF NANO-ZnO/PEG/PET COMPOSITE

Nano-ZnO particle （nZnOp） reinforced polyethylene glycol （PEG）/polyethylene terephthalate （PET） （nZnOp/PEG/PET） copolymeric composites with different mass fractions and molecular weights of PEG are synthesized via in-situ polymerization. The dispersion of nZnOp in copolymer matrixes and the effects of PEG and nZnOp particles on the crystallization behavior of the composites are studied by TEM, differential scanning calorimetry（DSC）, XRD and Fourier thansform infrared spectroscopy （FTIR ）. The results reveal that nZnOp particles are dispersed in the matrixes with nano-scale, and the addition of PEG induces more homogeneous dispersion of nZnOp. Simultaneously, these nanoparticles become nucleating centers during the crystallization of the matrixes. PEG segments can improve the flexibility of the PET molecular chain, resulting in the drop of the cold crystallization temperature and the rise of the crystallization rate of the composites. Furthermore, PEG （4 000） with the mass fraction of 10% can promote the crystallization rate of the composites. The mechanical properties show that the nano-particles strengthen and toughen the PET matrix, whereas PEG weakens these improve- ments.

Nano-Fe_(3)O_(4)强化牛粪厌氧发酵及抗性基因削减

为提高牛粪高浓度厌氧发酵产气性能,考察了不同浓度纳米四氧化三铁(Nano-Fe_(3)O_(4))对底物水解及产气效率的强化效果,探究其对发酵系统中微生物群落结构变化以及抗生素抗性基因(ARGs)归趋的影响.结果表明,添加500mg/L的Nano-Fe_(3)O_(4)可以提高牛粪高浓度厌氧发酵底物水解程度,增强系统稳定性,提高沼气产量12.36%.与对照相比,发酵系统中水解产酸菌厚壁菌门(Firmicutes)、纤维杆菌门(Fibrobacteres)的丰度分别显著增加了37.39%和75.86%.属水平上尤其是梭菌属(Clostridium)和瘤胃球菌(Ruminofilibacter)丰度是原来的3.50倍和8.69倍.产甲烷菌中甲烷八叠球菌(Methanosarcina)占主导地位,其丰度达2.55%,比对照显著增加27.50%.此外,潜在致病菌密螺旋体属(Treponema)和不动杆菌属(Acinetobacter)的丰度分别显著降低72.14%和93.69%;ARGs中四环素类(tetA、tetG、tetH、tetJ)、氨基糖苷类(aph(3)、aph(6))削减率达100%.磺胺酰胺类(sul1、sul2)平均削减率达74.41%~96.55%.研究表明添加适量的Nano-Fe_(3)O_(4)对稳定发酵系统、提高微生物活性、增加沼气产量、抗性基因削减等方面有多重促进作用,研究结果可为畜禽粪污沼气工程中Nano-Fe_(3)O_(4)等导电性外源调控添加剂的使用提供参考.

IN-SITU TEM OBSERVATION OF NANOSILICON FIBRE GROWTH

Nano silicon particles can be become nano fibre under low energy electron beam bombarding. The formation of the nano silicon fibre include two stages. At first, on the nano silicon particle surface many silicon atoms are gasified, then these silicon atoms deposit in the place where have more charge on account of the static electrical absorption and the point effect of the charge accumulation , these atoms grow into non crystalline silicon fibres. The second stage is the non crystalline silicon fibres crystallizing. Its crystallizing temperature is about 180℃. The growth mechanism of the nano silicon fibre is vapour solid mode.

TPU/Nano-ZnO复合改性沥青的性能研究及微观机制

为促进聚合物/纳米改性沥青在耐久性路面中的应用,在实验室将不同掺量的聚氨酯及纳米氧化锌添加到A-70#基质沥青中制备了复合改性沥青。采用传统物理性能试验、动态剪切流变试验(DSR)、弯曲梁流变试验(BBR)研究了其物理性能与流变特性,基于响应面法的优化设计来明确两种改性剂的最佳掺量。借助傅里叶红外光谱试验(FTIR)对其微观改性机理进行探讨。采用高压紫外汞灯环境箱对改性沥青进行不同时间的紫外老化,分析其抗紫外老化能力,并基于主成分分析法评价了老化性能测试指标的显著性。结果表明:聚氨酯与纳米氧化锌的共同作用提高了基质沥青的高温稳定性及低温抗裂性,两种改性剂的最佳掺量分别为5%、3%。根据FTIR结果,复合改性沥青的改性过程既存在物理共混,又有化学加成反应。聚氨酯及纳米氧化锌的加入在基质沥青紫外老化过程中能够抑制羰基、亚砜基等极性基团的生成,复数剪切模量、羰基指数、劲度模量及亚砜基指数对沥青紫外老化性能的影响最为显著。

抗菌PP/Rnano-ZnO复合材料的制备及性能研究

以棒状纳米氧化锌(Rnano-ZnO)为抗菌剂、聚丙烯(PP)为基材,采用熔融共混法在双螺杆挤出机中制备了抗菌PP/Rnano-ZnO复合材料。测试了复合材料的抗菌性能,通过DSC法研究了抗菌PP/Rnano-ZnO复合材料中Rnano-ZnO质量分数对结晶性能的影响,采用SEM分析了复合材料冲击断面的微观形貌,采用万能电子拉伸机测试了复合材料的力学性能。结果表明,抗菌PP/Rnano-ZnO复合材料中随着Rnano-ZnO的加入,结晶温度提高了1.81℃,相对结晶度提高了5.03%,冲击强度提高了47.83%,拉伸强度提高了20.96%和断裂伸长率提高了4790%;当抗菌PP/Rnano-ZnO复合材料中Rnano-ZnO质量分数为6.0%时,其力学性能、对大肠杆菌和金黄色葡萄球菌的抗菌效果最佳。

Preparation of Phenolic Resin/Silver Nanocomposites via in-situ Reduction

Resol type phenolic resin/silver nanocomposite was prepared by in-situ reduction method, in which the curing of phenolic resin and the formation of silver nano-particles took place simultaneously. The silver ions were reduced completely to silver nanoparticles, which were dispersed homogeneously in the resin matrix with narrow size distribution.

Dense copper azide synthesized by in-situ reaction of assembled nanoporous copper microspheres and its initiation performance

Copper azide with high density was successfully synthesized by in-situ reaction of nanoporous copper(NPC)precursor with HN_(3) gaseous.NPC with pore size of about 529 nm has been prepared by electroless plating using polystyrene(PS)as templates.The copper shells thickness of NPC was controlled by adjusting the PS loading amount.The effects of copper shell on the morphology,structure and density of copper azide were investigated.The conversion increased from 87.12%to 95.31%when copper shell thickness decrease from 100 to 50 nm.Meanwhile,the density of copper azide prepared by 529 nm NPC for 24 h was up to 2.38 g/cm^(3).The hollow structure of this NPC was filled by swelling of copper azide which guaranteed enough filling volume for keeping the same shape as well as improving the charge density.Moreover,HNS-IV explosive was successfully initiated by copper azide with minimum charge thickness of 0.55 mm,showing that copper azide prepared has excellent initiation performance,which has more advantages in the application of miniaturized explosive systems.

Modification of nano-TiO_2 by Al_2O_3 in-situ coating

A novel technology of in-situ coating Al2O3 on the surface of H4TiO4 was developed to prevent the aggregation of nano-TiO2 powders and improve the dispersibility and thermal stability in the way of forming a uniform coating layer. The heterogeneous nucleation was conducted to prepare the precursor of nano-TiO2 and then Al2O3 was coated on the surface of precursor. The effects of Al2O3 in-situ coating on the properties of nano-TiO2 were investigated. The results show that H4 TiO4 can be dispersed well under alkaline condition （pH 8. 5） and the heterogeneous nucleation can be controlled easily. The optimized uniform coating layer is obtained by adding 5 % （mass fraction ） and 10% of Al2O3 and the aggregation of nano-TiO2 powders is effectively inhibited and the dispersibility is obviously improved. The crystal sizes of TiO2 powders are 12.3, 11.4 and 8. 7 nm after coating 0, 5% and 10% of Al2O3 respectively. Al2O3 on the surface of particulates in amorphous phase could increase the thermal stability of nano-partieles after calcined at 550℃.

Platinum in-situ catalytic oleylamine combustion removal process for carbon supported platinum nanoparticles

Colloidal synthesis method such as oleylamine(OAm)-stabilized process is of great interest for obtaining uniform and highly dispersed platinum nanoparticle catalysts, yet the ligand may unavoidably inhibit their electro-catalytic performance. Thus, fully removing these ligands is critical to activate catalyst surface. Previous research of OAm removal process pointed that thermal annealing was the most effective way in comparison with other methods such as chemical washing, UV–Ozone irradiation and cyclic voltammetry sweeping, but generally resulting in undesired growth of platinum nanoparticle. Few studies concerning a more efficient ligand removal process have been published yet. In this work we proposed a platinum in-situ catalytic OAm combustion strategy to elucidate the removal mechanism of OAm ligands in thermal process and the key experimental parameters were also optimized. In addition, heat flow signal based on differential scanning calorimetry(DSC) measurement as a sensitive indicator, is suggested to reveal the ligand removal efficiency, which is much more reliable than the traditional spectroscopy.In comparison with commercial Pt/C sample, such a surface clean Pt/C electrocatalyst has shown an enhanced specific activity for oxygen reduction reaction. Our removal strategy and the evaluation method are highly instructive to efficient removal of different organic ligands.

In-situ magnetic field enhanced performances in ferromagnetic FeCo_(2)O_(4) nanofibers-based rechargeable Zinc-air batteries

Field-assisted electrocatalytic reactions are demonstrated to be sufficient strategies in enhancing the electrocatalyst activities for oxygen evolution reaction(OER).Here,we report the in-situ magnetic field enhanced electrocatalytic activity in ferromagnetic FeCo_(2)O_(4)nanofibers.Our results demonstrate that the overpotential of FeCo_(2)O_(4)nanofibers at 10 mA cm^(-2)shows a left-shift of 40 mV for the OER by applying an external magnetic field,and no obvious change has been observed in the non-ferromagnetic-order Co3O4nanofibers.Calculation results indicate that there are more overlaps between the density of states for Co3d and O 2p by applying an external magnetic field.Accordingly,the spin hybridization of 3d-2p and the kinetics of spin charge transfer are optimized in ferromagnetic FeCo_(2)O_(4),which can promote the adsorption of oxygen-intermediates and electron transfer,significantly improving its electrocatalytic efficiency.What’s more,the maximum power density of the FeCo_(2)O_(4)nanofibers based Zn-air battery(ZAB)increases from 97.3 mW cm^(-2)to 108.2 mW cm^(-2)by applying an external magnetic field,providing a new idea for the application of magnetic cathode electrocatalysts in ZABs.

In-situ incorporation of halloysite nanotubes with 2D zeolitic imidazolate framework-L based membrane for dye/salt separation

Layered assembled membranes of 2D leaf-like zeolitic imidazolate frameworks(ZIF-L)nanosheets have received great attention in the field of water treatment due to the porous structure and excellent antibacterial ability,but the dense accumulation on the membrane surface and the low permeate flux greatly hinder their application.Herein,we synthesized m HNTs(modified halloysite nanotubes)/ZIF-L nanocomposites on modified m HNTs by in situ growth method.Interestingly,due to the different size of m HNTs and ZIF-L,m HNTs were packed in ZIF-L nanosheets.The hollow m HNTs provided additional transport channels for water molecules,and the accumulation of the ZIF-L nanosheets was decreased after assembling m HNTs/ZIF-L nanocomposites into membrane by filtration.The prepared m HNTs/ZIF-L membrane presented high permeate flux(59.6 L·m^(-2)·h^(-1)),which is 2-4 times of the ZIF-L membranes(14.8 L·m^(-2)·h^(-1)).Moreover,m HNTs/ZIF-L membranes are intrinsically antimicrobial,which exhibit extremely high bacterial resistance.We provide a controllable strategy to improve 2D ZIF-L assembles,and develops novel membranes using 2D package structure as building units.

In-situ hydrocarbon formation and accumulation mechanisms of micro- and nano-scale pore-fracture in Gulong shale, Songliao Basin, NE China

By conducting experimental analyses, including thermal pyrolysis, micro-/nano-CT, argon-ion polishing field emission scanning electron microscopy (FE-SEM), confocal laser scanning microscopy (CLSM), and two-dimensional nuclear magnetic resonance (2D NMR), the Gulong shale oil in the Songliao Basin was investigated with respect to formation model, pore structure and accumulation mechanism. First, in the Gulong shale, there are a large number of pico-algae, nano-algae and dinoflagellates, which were formed in brackish water environment and constituted the hydrogen-rich oil source materials of shale. Second, most of the oil-generating materials of the Qingshankou Formation shale exist in the form of organo-clay complex. During organic matter thermal evolution, clay minerals had double effects of suppression and catalytic hydrogenation, which expanded shale oil window and increased light hydrocarbon yield. Third, the formation of storage space in the Gulong Shale was related to dissolution and hydrocarbon generation. With the diagenesis, micro-/nano-pores increased, pore diameter decreased and more bedding fractures appeared, which jointly gave rise to the unique reservoir with dual media (i.e. nano-scale pores and micro-scale bedding fractures) in the Gulong shale. Fourth, the micro-/nano-scale oil storage unit in the Gulong shale exhibits independent oil/gas occurrence phase, and shows that all-size pores contain oils, which occur in condensate state in micropores or in oil-gas two phase (or liquid) state in macropores/mesopores. The understanding about Gulong shale oil formation and accumulation mechanism has theoretical and practical significance for advancing continental shale oil exploration in China.

In-situ Characterization of Non-aqueous Nano-dispersion Systems by Freeze-etching TEM and Comparative Study with Laser Scattering Method

In-situ characterization of non-aqueous nano-dispersion systems（NANDS） by freeze-etching transmission electron microscope（FETEM） was reported.To improve just-for-once successive rate of specimen preparation and get good characterization results,an improving specimen preparation method of freezing etching was developed.Size,distribution and morphology of NANDS were directly visualized.Some information of particle dispersion feature and particle density can also be obtained.Reproductivity of the FETEM characterization is excellent.Comparing with laser scattering method,which is liable to give positive error especially for small size particle anchoring disperser,FETEM characterization can give more accurate measurement of particle size.Moreover,FETEM can give dispersion feature of nanoparticle in non-aqueous medium.

SYNTHESIS AND CHARACTERIZATION OF POLYPROPYLENE/MONTMORILLONITE NANOCOMPOSITES VIA AN in-situ POLYMERIZATION APPROACH

Polypropylene/montmorillonite (PP/MMT)nanocomposites were prepared by in-situ polymerization using aMMT/MgCl_2/TiCl_4-EB Ziegler-Natta catalyst activated by triethylaluminum(TEA). The enlarged layer spacing of MMT wasconfirmed by X-ray wide angle diffraction (WAXD), demonstrating that MMT were intercalated by the catalyst components.X-ray photoelectron spectrometry (XPS) analysis proved that TiCl_4 was mainly supported on MgCl_2 instead of on the surfaceof MMT The exfoliated structure of MMT layers in the PP matrix of PP/MMT composites was demonstrated by WAXDpatterns and transmission electron microscopy (TEM) observation. The higher glass transition temperature and higher storage modulus of the PP/MMT composites in comparison with pure PP were revealed by dynamic mechanical analysis (DMA).