Preparation of nanometer δ- and β-bismuth trioxide by vacuum vapor-phase oxidation

A stable δ- and β-bismuth trioxide was prepared at room temperature by vacuum vapor-phase oxidation. The average crystal size of products was 14.6 nm (by XRD), the d(0.5) value was in the range from 62 nm to 69 nm, and geometric standard deviation(GSD) was from 1.42 to 1.64. The results show that δ-Bi2O3 is formed when quenching rates is rapid and β-Bi2O3 is formed when it is slow. The size of grains increases with rising reaction temperature, flow rate of carrier gas, residual pressure of system and longer growing time of grains.

EFFECT OF VACUUM HEAT TREATMENT ON OXIDATION BEHAVIOR OF SPUTTERED NiCrAlY COATING

A bond coat for thermal barrier coating (TBC), NiCrAlY coating, is subjected to vac-uum heat treatment in order to remove internal stress before ceramic top coat is de-posited. The effect of vacuum heat treatment on the oxidation behavior of the sputtered NiCrAlY coating has been investigated. The as-sputtered NiCrAlY coating consists of γ-Ni and b-NiAl phases. After vacuum heat treatment, the sputtered NiCrAlY coating mainly consists of γ'-Ni3Al, β-NiAl, γ-Ni, and trace of α-Al2O3 phases. The isothermal oxidation of sputtered NiCrAlY coating with and without vacuum heat treatment has been performed at 1000℃. It is shown that a-Al2O3 formed during vacuum heat treatment acts as nuclei for the formation of a-Al2O3, and the protective a-Al2O3 scale is formed more rapidly on the vacuum heat treated NiCrAlY coating than that formed on the untreated coating. Also the a-Al2O3 scale has a better adherence to the vacuum heat treated NiCrAlY coating. Therefore the vacuum heat treatment improves the oxidation resistance of sputtered NiCrAlY coating.

Effect of Y_2O_3 on microstructure and oxidation of γ-Ni+γ′-Ni_3Al coatings transformed from electrodeposited Ni-Al films at 1000℃

The electrodeposited Y2O3-dispersedγ-Ni+γ′-Ni3Al coatings on Ni substrates were developed by the conversion of electrodeposited Ni-Al-Y2O3 films with dispersed Al microparticles in Ni matrix into Ni3Al by vacuum annealing at 800℃for 3 h. For comparison,Y2O3-freeγ-Ni+γ′-Ni3Al coatings with a similar Al content were also prepared by vacuum annealing the electrodeposited microparticle-dispersed composite coatings of Ni-Al under the same condition.SEM and TEM characterizations show that the electrodeposited Y2O3-dispersedγ+γ′coatings exhibit finer grains,a more homogeneous distribution ofγ′,and a narrowedγ′phase spacing compared with the electrodeposited Y 2 O3-freeγ+γ′coatings.The oxidation at 1 000℃shows that the addition of Y2O3 significantly improves the oxidation resistance of the electrodepositedγ+γ′coatings.The effect of Y2O3 particles on the microstructure and oxidation behavior of the electrodepositedγ+γ′coatings was discussed in detail.

Use of various MgO resources for high-purity Mg metal production through molten salt electrolysis and vacuum distillation

A green and effective electrolytic process was developed to produce high-purity Mg metal using primary and secondary resources containing Mg O as a feedstock. The electrolysis of various Mg O resources was conducted using a Cu cathode in MgF2– LiF – KCl molten salt at 1043 K by applying an average current of 1.44 A for 12.5 h. The electrolysis of calcined North Korean magnesite and seawater Mg O clinker yielded Mg alloys of MgCu2and(Cu) phases with current efficiencies of 89.6–92.4%. The electrolysis of oxidized Mg O-C refractory brick, aged ferronickel slag, and ferronickel slag yielded Mg alloys of MgCu2and(Cu) phases with current efficiencies of 59.3–92.3%. The vacuum distillation of Mg alloys obtained was conducted at 1300 K for 10 h to produce high-purity Mg metal. After vacuum distillation, Mg metal with a purity of above 99.994% was obtained. Therefore, this study demonstrates the feasibility of the production of high-purity Mg metal from various Mg O resources using a novel electrolytic process with a Cu cathode, followed by vacuum distillation.

High Temperature Sintering and Oxidation Behavior in Plasma Sprayed TBCs [Single Splat Studies] Paper 1—Role of Heat Treatment Variations

The TBC system is examined with regards to its response to thermal exposure at high temperature. It has been established before that the thermally grown oxide (TGO) layer that forms upon bond coat oxidation is the key factor determining the performance of the TBC system and/or its failure. However, characteristics of TGO growth, bond coat rumpling, principles governing failure of TBC systems and the various failure mechanisms have been studied extensively in case of just super alloy with bond coat or with thick top coating. In this study super alloy/bond coat system with single splats of YSZ instead of thick topcoat is analyzed in order to scrutinize the effect on the first layer of splats during thermal exposure. The splats with microcracks are the building blocks of the top coat. The most important aspect of this layer is the inherent inter-splat and intra-splat porosity which undergoes sintering during thermal exposure. The interactions between the YSZ splats and the evolving TGO is directly linked to the presence or absence of bond coat oxidation. Therefore the high temperature behavior of this system is analyzed with variations in heat treatment involving, temperature, duration and environment of thermal exposure.

High Temperature Sintering and Oxidation Behavior in Plasma Sprayed TBCs [Single Splat Studies] Paper 2—Relevance of Variation in Materials Systems of TBC Components

The TBC system’s response to thermal exposure at high temperature is discussed here. The relevance of the microstructural aspects of each component of the TBC system is emphasized. The top coat is a YSZ ceramic coating consisting of a collection of splats on top of one another. The most important aspect of this layer is the inherent inter-splat and intra-splat porosity which undergoes sintering during thermal exposure. This study investigates the effect of thermal exposure on the microstructure and sintering behavior in single splats produced using different starting powders since this has been shown to influence the basic microstructure of YSZ topcoat. The bond coat is an MCrAlY metallic coating which serves as an Al reservoir and allows the formation of a protective alumina, Thermally Grown Oxide (TGO) layer between the bond coat (BC) and the top coat (TC) layers. This oxide scale formed upon thermal exposure prevents further oxidation of the underlying component (substrate) and thus provides protection. As such, the content of free Al in the bond coat layer is of significance and makes it crucial to understand the influence of bond coat microstructure evolution and oxidation involved during its formation. The interaction between the bond coat, the TGO and the top coat layers is examined in this study to understand the high temperature behavior of the TBC system with regards to variations in the top coat and bond coat material systems used.

Production of high-purity Mg metal from dolomite through novel molten salt electrolysis and vacuum distillation

In this study,a novel Mg production process for producing high-purity Mg metal from dolomite was developed.When the electrolysis of calcined dolomite was conducted using Cu cathode and C anode in MgF_(2)–LiF molten salt at 1083–1173 K by applying an average current of 1.42–1.46 A for 9.50–21.0 h,the current efficiency of 66.4–88.6%was obtained.The produced Mg alloys consisted of MgCu_(2)and Cu(Mg)or MgCu_(2)and CuMg_(2)phases,depending on the Mg concentration in the Mg alloy.When the electrolysis of calcined dolomite was conducted in MgF_(2)–LiF–CaF_(2)molten salt at 1083 K,the current efficiency was 40.9–71.4%,owing to undesired reactions such as electroreduction of Ca^(2+)or/and CO_(3)^(2−)ions.Meanwhile,the current efficiency increased from 40.9%to 63.2%by utilizing a Pt anode,because the occurrence of CO_(3)^(2−)ions in the molten salt was prevented.After vacuum distillation of the obtained Mg alloys at 1300 K for 10 h,Mg metal with a purity of 99.9996–99.9998%was produced.Therefore,the feasibility of this novel process for the production of high-purity Mg metal from dolomite was demonstrated.

铺层方式对VIHPS制备的GO-CF混杂增强复合材料弯曲性能的影响

本文首先采用真空浸渗热压工艺(VIHPS)制备了不同铺层方式的氧化石墨烯-碳纤维(GO-CF)混杂增强复合材料,并对该材料进行三点弯曲试验,再通过扫描电子显微镜(SEM)表征其微观断口形貌。然后使用Digmat软件的FE模块建立微-纳跨尺度的代表性体积单元(RVE)模型,将该模型导入ANSYS Workbench软件中进行三点弯曲仿真模拟。复合材料三点弯曲试验结果表明,随着沿试样宽度方向(Y向)纤维铺层的增加,复合材料的弯曲强度从433.2 MPa降低至12.7 MPa,弯曲模量从13.8 GPa降低至0.2 GPa,它们分别降低了97.07%和98.55%。最后通过对比试验与仿真结果发现,两种结果的变化趋势基本一致,且仿真结果与试验结果接近。复合材料在弯曲变形过程中,受到拉伸和压缩的共同作用,其中导致复合材料失效的方式主要包括基体开裂、界面脱粘和纤维断裂。

真空冷冻干燥肉苁蓉工艺的研究

为了研究肉苁蓉产地趁鲜切制干燥的可行性,采用真空冷冻干燥法,通过单因素试验比较了肉苁蓉冻干过程中片状、粒状、粉状等不同切制方式对其干燥率及质量的影响,为肉苁蓉的干燥保存提供有效可行的加工方法;使用HPLC-UV方法,对粉状肉苁蓉药材中的松果菊苷和毛蕊花糖苷进行测定。结果表明,通过粉状切制的肉苁蓉产品干燥率及质量最好;粉状的切制方式所得的肉苁蓉放置1年后,松果菊苷和毛蕊花糖苷含量较高;小块状的处理方式最为简易,产品的干燥率也较为优秀,氧化程度在3种制备方式中最低。

超声分散时间对GO-CF增强SMPC形状记忆性能的影响

为了研究超声分散时间对形状记忆聚合物复合材料(SMPC)微观组织和形状记忆性能的影响,采用真空浸渗热压工艺制备6组不同超声分散时间的GO-CF混杂增强SMPC,通过扫描电子显微镜表征SMPC的微观组织形貌,开展形状记忆性能的测试.结果表明,适当的超声分散时间可以将GO剥离成片状结构并均匀分散在SMPC中,形成机械联锁和化学键合.随着超声分散时间的增加,SMPC的形状固定率和形状回复率呈现先增大后减小的趋势,除30 min外,其他SMPC的平均回复速率呈现先减小后增大的趋势,当超声分散60 min时,SMPC具有最佳的形状记忆性能,形状固定率和形状回复率分别达到97.85%和97.30%,最大回复力为10.47 N,平均形状回复速率为1.04°/s,机械联锁和化学键合这种复合结构的增加有利于增强SMPC的形状记忆性能,但需要更多的能量来实现SMPC的形状回复.

Copper nanowires decorated with TiO_(2−x) from MXene for enhanced electrocatalytic nitrogen oxidation into nitrate under vacuum assistance

The green synthesis of nitrate(NO_(3)^(−))via electrocatalytic nitrogen oxidation reaction(NOR)is a promising strategy for artificial nitrogen fixation,which shows great advantages than traditional nitrate synthesis based on Haber–Bosch and Ostwald processes.But the poor N_(2)absorption,high bond energy of N≡N(941 kJ·mol^(−1)),and competing multi-electron-transfer oxygen evolution reaction(OER)limit the activity and selectivity.Herein,we fabricated MXene-derived irregular TiO_(2)−x nanoparticles anchored Cu nanowires(Cu-NWs)electrode for efficient electrocatalytic nitrogen oxidation,which exhibits a NO_(3)−yield of 62.50μg·h^(−1)·mgcat^(−1)and a Faradaic efficiency(FE)of 22.04%,and a significantly enhanced NO_(3)−yield of 92.63μg·h^(−1)·mgcat^(−1),and a FE of 40.58%under vacuum assistance.The TiO_(2)−x/Cu-NWs electrode also shows excellent reproducibility and stability under optimal experimental conditions.Moreover,a Zn-N_(2)reaction device was assembled with TiO_(2−x)/Cu-NWs as an anode and Zn plate as a cathode,obtaining an extremely high NO_(3)−yield of 156.25μg·h^(−1)·mgcat^(−1).The Zn-nitrate battery shows an open circuit voltage(OCV)of 1.35 V.This work provides novel strategies for enhancing the performance of ambient N_(2)oxidation to obtain higher NO_(3)^(−)yield.

双碱法脱硫工艺提标改造与实践

介绍了淄博铁鹰球团制造有限公司双减法脱硫工艺技术改造过程和应用实践。通过对脱硫工艺的石灰浆液制备及输送系统、SO_(2)吸收系统、石膏脱水系统、工艺水系统、电气及自动控制系统等关键环节技术创新与改造,有效解决了脱硫能力不足、压滤效果差、塔体及喷淋管路结晶严重、工艺水平衡困难等运行难题,并实现了由双减法向石灰-石膏法脱硫工艺过渡,满足了生产需要,降低了脱硫运行成本。

Synthesis of a new ordered mesoporous NiMoO_4 complex oxide and its efficient catalytic performance for oxidative dehydrogenation of propane

Highly ordered mesoporous NiMoO4 material was successfully synthesized using mesoporous silica KIT-6 as hard template via vacuum nanocasting method. The structure was characterized by means of XRD, TEM, N2 adsorption-desorption, Raman and FT-IR. The mesoporous NiMoO4 with the coexistence of a-NiMoO4 and fl-NiMoO4 showed well-ordered mesoporous structure, a bimodal pore size distribution and crystalline framework. The catalytic performance of NiMoOa was investigated for oxidative dehydrogenation of propane. It is demonstrated that the mesoporous NiMoO4 catalyst with more surface active oxygen species showed better catalytic performance in oxidative dehydrogena- tion of propane in comparison with bulk NiMoO4.

Preparation of Nano-composites Membranes with Graphic Oxides and Polylactic Acid

Organic polymer materials were used as a layer of adhesive into the graphene sheet between the layers to enhance the interaction force between the nano-structure to achieve excellent mechanical properties and barrier properties. PLA with good flowability and easy processing was selected. The mechanical properties and barrier properties of the graphene-based composites were improved by the use of PLA for good flowability, making it easy to enter the GO layer as a binder. Three methods of preparation of GO/PLA homogeneous composite membranes were designed by vacuum filtration. The experimental results show that the injection of PLA as a molecular binder into the GO layer can effectively mimic the nano-structure, and enhance the intergranular force of the graphene molecules and the compatibility with the polymer matrix.

Development of a novel electrolytic process for producing high-purity magnesium metal from magnesium oxide using a liquid tin cathode

The current electrolytic processes for magnesium(Mg)metal have several disadvantages,such as anhydrous magnesium chloride(MgCl_(2))preparation and generation of harmful chlorine(Cl_(2))gas.To overcome these drawbacks,a novel Mg production process to produce high-purity Mg metal directly from magnesium oxide(MgO)was investigated in this study.The electrolysis of MgO was conducted using a liquid tin(Sn)cathode and a carbon(C)anode in the eutectic composition of a magnesium fluoride(MgF_(2))-lithium fluoride(LiF)molten salt under an applied voltage of 2.5 V at 1053-1113 K.Under certain conditions,the Mg-Sn alloys with Mg_(2)Sn and Mg(Sn)phases were obtained with a current efficiency of 86.6%at 1053 K.To produce high-purity Mg metal from the Mg-Sn alloy,vacuum distillation was conducted at 1200-1300 K for a duration of 5-10 h.Following the vacuum distillation,the concentration of Mg in the Mg-Sn alloy feed decreased from 34.1 to 0.17 mass%,and Mg metal with a purity of 99.999%was obtained at 1200 K.Therefore,the electrolytic process developed here is feasible for the production of high-purity Mg metal from MgO using an efficient method.

Double oxide film defects in Ni-based super-alloy castings

A new class of defects has been recently discovered,which are regarded double oxide film defects.In this study, a number of Ni-based vacuum-cast test bars were investigated. The fractures in the broken test barswere observed by Scanning Electron Microscopy (SEM). Energy Dispersive Spectroscopy (EDS), as well asWavelength Dispersive Spectroscopy (WDS) were used to characterize the chemical elements of the fracture'ssurface. Observation by SEM revealed the presence of inclusions identified as films that appeared to have initiatedthe growth of carbides. This study has added to the evidence that oxide film defects do exist in Ni-based super-alloyin certain vacuum casting conditions. It provides a reference for researchers' further study on the defects, andprovides a possible direction for researchers to improve casting technology so as to remove these defects.

真空紫外活化亚硫酸盐在有氧条件下降解二甲双胍

以治疗Ⅱ型糖尿病的基础药物——二甲双胍(MET)为研究对象,考察其在真空紫外(VUV)活化亚硫酸盐有氧(VUV/SO_(3)^(2-)/O_(2))体系中的降解效果。通过淬灭试验,验证了反应体系中硫酸盐自由基(SO_(4)^(-)·)、羟基自由基(HO·)、水合电子(e-aq)和氢离子自由基(·H)活性物质的存在,同时考察VUV/SO_(3)^(2-)/O_(2)体系中pH、亚硫酸盐(SO_(3)^(2-))浓度、光强、天然有机物(NOM)和常见无机离子对MET降解的影响。结果表明VUV/SO_(3)^(2-)/O_(2)体系对MET的降解效果明显优于VUV/O_(2)或SO_(3)^(2-)/O_(2)体系,在180 min内可降解91%的MET;MET降解率随pH的增大先上升后下降,随SO_(3)^(2-)浓度和光强的增加而增加;NOM、HCO_(3)^(-)、Cl^(-)和NH+4的加入对MET降解均起到抑制作用。共检测到6种降解产物,推测MET共有3条降解路径,产物主要经过C—N键断裂、去甲基化、脱氨基化、环化和脱氢等反应得到。

粗锡绿色短流程精炼

针对传统粗锡精炼技术存在的工艺流程长、杂质脱除难、环境影响大等问题,提出“凝析离心-氧化除杂-连续结晶-真空挥发”粗锡精炼新技术思路。系统开展了粗锡凝析离心除铁砷、氧化除铜镍锑、连续结晶除银、真空挥发除铅铋的理论研究,阐明杂质组元固-液-气相间的迁移和分布规律,并进行小型实验、半工业实验和工业实验。实验结果表明,粗锡绿色短流程精炼新技术可生产纯度为99.99%的精锡,精锡品质达到国标4N锡要求。与传统粗锡精炼技术相比,粗锡绿色短流程精炼新技术具有原料适应性强、辅料消耗少、“三废”排放少、锡直收率高、渣率低、综合能耗低、生产成本低等优点。

真空提取核桃粕多酚的抗氧化活性研究

目的 探究真空提取的核桃粕(walnut meal)多酚的抗氧化活性。方法 以非真空条件下提取的多酚为对照,采用超声波辅助真空法提取核桃粕多酚,用HPD-100型大孔树脂对多酚进行纯化,福林酚(Folin-Ciocalte)法测定多酚含量,通过试剂盒检测多酚对1,1-二苯基-2-苦基肼自由基(1,1-diphenyl-2-picrylhydrazyl,DPPH)、超氧阴离子自由基的清除率及Fe3+还原能力(ferric reducing antioxidant power,FRAP)来评价其体外抗氧化活性,用cck8(cell countingkit-8)法测定不同浓度的核桃粕多酚对HepG2细胞的毒性作用,确定3个无毒性作用浓度,以770μmol/L的H_(2)O_(2)诱导HepG2细胞建立氧化应激损伤模型,通过测定HepG2细胞中丙二醛(malonicdialdehyde, MDA)含量、超氧化物歧化酶(superoxide dismutase, SOD)活力、谷胱甘肽(glutathione, GSH)含量探究12.5、25.0、50.0μg/mL核桃粕多酚对HepG2细胞氧化损伤的保护作用。结果 真空条件下提取的多酚含量为26.96mg/g,比非真空条件下提取的多酚含量高出14.50%;经HPD-100型大孔树脂纯化后,对照组和真空组核桃粕多酚纯度分别由22.69%、26.60%提高至73.87%、77.53%;纯化后,对照组与真空组多酚质量浓度为0.5 mg/mL时对DPPH自由基的清除率高达93.83%、93.67%,高于维生素C的清除率91.03%;同一浓度范围内,真空条件下提取的核桃粕多酚对超氧阴离子自由基的清除率和FRAP均显著高于对照组多酚(P<0.05),其中多酚质量浓度为2.0 mg/mL时,对照组与真空组多酚的FRAP分别为8.91μmol/L、9.92μmol/L,均高于维生素C的FRAP(7.91μmol/L);核桃粕多酚可以使受氧化损伤的HepG2细胞内MDA含量明显减少,并能提高受氧化损伤细胞内SOD活力及GSH含量。结论 真空条件有利于核桃粕多酚的提取,提取纯度较高,纯化后核桃粕多酚具有较好的体外氧化活性,对HepG2细胞氧化损伤有一定的保护作用。

包装方式对即食真空油炸带鱼贮藏品质的影响

本文通过研究不同包装的即食真空油炸带鱼在25℃贮藏60 d过程中的品质变化来筛选合适的包装材料。分别采用封罐包装和铝箔袋充氮包装,考察贮藏过程中真空油炸带鱼水分含量、水分活度、pH、过氧化值(Peroxide value,POV)、硫代巴比妥酸值(Thibarbituric acid reactive substances,TBARS)、酸价(Acid value,AV)的变化,并测定贮藏终点即食真空油炸带鱼的滋味物质。结果表明:真空油炸带鱼在贮藏过程中水分含量,水分活度呈现先增加后趋于平稳的趋势,贮藏60 d时封罐包装的水分含量,水分活度分别是铝箔袋充氮包装的1.23倍,1.19倍;贮藏过程中脂质氧化的相关参数(POV、TBARS、AV)呈现时间依赖性上升趋势,贮藏60 d时封罐包装的POV、TBARS、AV分别是铝箔袋充氮包装的1.84倍,1.43倍和1.13倍。因此铝箔袋充氮包装可以有效阻隔环境中的水分进入包装和减缓产品脂质氧化劣变;通过电子舌测定贮藏终点即食真空油炸带鱼的滋味物质,得出铝箔袋充氮包装可以在减缓苦味物质生成的同时在咸味、鲜味、丰富性方面优于封罐包装。综上所述,铝箔袋充氮包装是更有利于即食真空油炸带鱼包装和贮藏的包装材料。