Electron theory analysis about the influence of Cr and Mn on the carbide spheroidization by heat treatment

It is found that the distribution of covalent electron pair number and covalent bond energy was nonuniform in carbides Fe 3C, (Fe,Cr) 3C and (Fe,Mn) 3C, in which the energy difference between the strongest and the weakest bonds is very great. A criterion of covalent bond breaking during the heat treatment of M 3C pattern carbide is presented as follows. If the heat energy \%E\-\%w from heat treatment is higher than the diffusion activation energy \%Q\% of carbon atom in γ_Fe, the less the covalent bond energy \%E\% α is, the earlier the covalent bond α will be broken. According to the criterion, why the breaking of (Fe,Mn) 3C network was easier than that of Fe 3C network and why the breaking of (Fe, Cr) 3C network was more difficult than that of Fe 3C network are explained. It is indicated that Mn promoted the carbide to be spheroidized and Cr hindered the carbide from spheroidization during the heat treatment of carbides spheroidization.     

Synthesis of boron-doped diamond with laser heated diamond anvil cell

Boron-doped diamond has been synthesized from graphite mixed with different ratio of B₄C at high pressure high temperature (HPHT) using laser heated diamond anvil cell. The starting composition was transformed to diamond compound at pressure ∼9 GPa, 2300–2400 K as indicated by the in-situ X-ray diffraction pattern with synchrotron radiation source. Raman spectrum of the recovered specimen from HPHT state confirmed that boron has been doped into diamond lattice.     

Synthesis of γ-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript>/Au magnetic composites for immobilization of bovine serum albumin

A method for the two-step synthesis of magnetic composites with a γ-Fe₂O₃ core, silica inner layer and numerous gold nanoparticles supported on the surface of the silica (γ-Fe₂O₃/SiO₂/Au) is described. First, thiol-functionalized γ-Fe₂O₃/SiO₂ composites and gold colloids are prepared by modifying γ-Fe₂O₃/SiO₂ composites with mercaptosilane and reduction of Au³⁺ to Au⁰ with citrate, respectively. Gold nanoparticles are then assembled on the surface of the thiol-functionalized γ-Fe₂O₃/SiO₂ composites to form γFe₂O₃/SiO₂/Au composites. The structure of the composite particles is confirmed by transmission electronic microscopy and powder X-ray diffraction. Immobilization studies with bovine serum albumin (BSA) demonstrate that the γ-Fe₂O₃/SiO₂/Au composites can be used to immobilize BSA, making them useful for biomedical and biological applications.     

真空条件下钎焊单层金刚石砂轮的研究

单层高温钎焊超硬磨料砂轮具有电镀砂轮无法比拟的优异磨削性能。在真空条件下用Ni-Cr合金做钎料进行了钎焊单层金刚石砂轮的实验研究,实现了金刚石与钢基体间牢固的化学冶金结合。扫描电镜X射线能谱,结合X射线衍射结构分析发现,在金刚石界面上有Cr的碳化物Cr3C2和Cr7C3存在,而钢基体结合界面上则生成有(FexCry)C,这应是金刚石与钢基体之间具有较高结合强度的主要原因,通过磨削实验验证了金刚石确实有很高的把持强度。     

Catalyst enhanced chemical vapor deposition of nano-particle nickel films on teflon surface

Films formed with nanosized nickel particles on teflon surface were prepared by means of catalyst enhanced chemical vapor deposition (CECVD) with Ni(dmg)₂, Ni(acac)₂, Ni(hfac)₂, Ni(TMHD)₂, and Ni(cp)₂ as precursors, and complexes Pd(hfac)₂, PdCl₂ and Pd(η ³-2-methylallyl)acac as catalyst under carrier gas (H₂). The film growth rate depends on the precursors and substrate temperature. The chemical value, purity and surface morphology of the Ni particle films were characterized by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The films obtained were shiny with silvery color, and consisted of grains with a particle size of 50–140 nm. The Ni was metallic of which the purity was about 90%–95% from XPS analysis. SEM micrograph showed that the film had good morphology.      

动态催化聚合C3N4膜的研究

自Ｃｏｈｅｎ等人[1] 揭示β Ｃ3Ｎ4 的结构和性质以来 ,实验聚合沉积 β Ｃ3Ｎ4 膜的工作一直继续进行着 .早期的工作[2～ 10 ] 大多数采用气相沉积 ,工作气体一般是ＣＨ4 Ｎ2 或ＣＨ4 ＮＨ3,由于金刚石、石墨和Ｃ3Ｎ4 中Ｃ( 1ｓ)的结合能非常接近 ,在聚合反应时因相互竞争 ,其沉积产物常常是无定形碳、石墨、金刚石和Ｃ3Ｎ4 的混合物 .而在Ｃ3Ｎ4 聚合物中 ,常常包含有β Ｃ3Ｎ4 ,α Ｃ3Ｎ4 和石墨结构型Ｃ3Ｎ4 .Ｃｈｅｎ等人[11] 提出 ,采用适宜的有机分子预聚体 ,ＹｏｕＪｉ ｔａｎｉ等人[10 ] 提出采用不含Ｃ≡Ｎ的有机分子预聚体 ,…     

Study on growth of coarse grains of diamond with high quality under HPHT

The growth of coarse grains of diamond was observed with graphite as carbon source and Fe₈₀Ni₂₀ alloy powder as catalyst at HPHT in a China-type SPD 6×1670T cubic high-pressure apparatus with highly exact control system. To synthesize coarse grains of diamond crystal with high quality, advanced indirect heat assembly, powder catalyst technology and catalyst with optimal granularity were used. Especially the nucleation of diamond and the growth rate were strictly controlled by the optimized synthesis craft. At last, diamond crystals (about 0.85 mm) in the perfect hex-octahedron shape were successfully synthesized at ~5.4 GPa and ~1360℃ in 60 min. The characteristic of crystal growth with powder catalyst technology under HPHT was discussed. The results and techniques might be useful for production of coarse grains of diamond.     

复合金刚石薄膜的介电特性

利用热丝大面积金刚石薄膜气相合成（CVD）装备制备了复合金刚石薄膜，并对其表面和断面分别进行了扫描电镜（SEM），原子力显微镜（AFM）和Raman光谱表征，研究了该复合结构的介电性能，利用共振电路测量了高频下薄膜的介质损耗与频率的关系，结果表明，复合结构由普通多晶金刚石薄膜和纳米金刚石薄膜组成，薄膜的表层结构体现了纳 米金刚石的特征，复合金刚石薄膜不仅具有表面光滑的优点，介电性能也接近于常规的多晶金刚石薄膜，是一种较好的电子材料，可应用于金刚石薄膜半导体器件的制备。     

Low-field positive and high-field negative magnetoresistances in multiphase Fe-oxide thin films at room temperature

Multiphase Fe-oxide thin films are fabricated on glass substrates by a facing-target sputtering tech- nique. X-ray diffraction and X-ray photoelectron spectroscopy reveal that Fe, Fe3BO4, γ -Fe2BO3B and FeO coexist in the films. High resolution transmission electron microscopy shows the well-defined colum- nar grain structure with the unoxidized Fe as the core and iron-oxide as the shell. The low-field positive and high-field negative magnetoresistances coexist in such a system at room temperature, which can be explained by considering a shell/core model. Nonlinear current-voltage curve and photovoltaic effect further confirm the tunneling-type conduction.     

Magnetic field induced synthesis of (Ni,Zn)Fe2O4 spinel nanorod for enhanced alkaline hydrogen evolution reaction

Recently, the introduction of external fields(light, thermal, magnetism, etc.) during electrocatalysis reactions gradually becomes a new strategy to modulate the catalytic activities. In this work, an external magnetic field was innovatively employed for the synthesis progress of(Ni, Zn)Fe₂O₄spinel oxide(M-(Ni, Zn)Fe₂O₄). Results indicated the magnetic field(≤250 m T) would affect the morphology of catalyst due to the existing Fe ions, inducing the M-(...     

在MgO(001)基板上生长连续的L10-FePt 纳米薄膜

用磁控溅射法在加热到400℃的MgO(001)基片上沉积了总厚度为25 nm 的[Fe(0.6 nm)/Fe_30.5Pt_69.5(1.9nm)]₁₀ 多层连续薄膜, 并对其在[500, 900]℃的温度范围进行了3h 的真空热处理. 结果表明, 薄膜在沉积过程中发生了层间扩散, 形成A1 相的FePt 合金, 表现为软磁特性; 热处理温度高于700℃时, 薄膜内形成L1₀ 相的(001)织构, 其单轴磁晶各向异性能高于2.5×10⁷ erg cc^-1; 薄膜能在800℃以下保持形貌连续. 借助于半导体载流子扩散和复合模型, 对薄膜在高温下形貌保持连续的机理进行了探讨. 分析认为, 虽然薄膜在沉积过程中发生了层间扩散, 但内部仍然残存微弱的周期性成分起伏, 这可以有效阻碍热处理过程中因相变而引起的Pt 元素析出, 从而抑制了因形成富Pt 晶界而导致的形貌不连续. 这种薄膜可以方便地用于微加工制作磁性阵列和隧道结.     

镍基合金CMSX-4在3.5wt.% NaCl溶液中的腐蚀行为

研究二代镍基合金CMSX-4在质量分数为3.5% NaCl溶液中的腐蚀行为,对该类合金在海洋性环境条件下的应用具有深远意义。通过动电位极化方法研究室温条件下镍基合金CMSX-4在3.5 wt.% NaCl溶液中的电化学行为,利用扫描电子显微镜（SEM）、能谱分析仪（EDS）和X射线光电子能谱仪（XPS）对合金表面阳极腐蚀产物进行微观形貌观察及成分分析。研究表明,CMSX-4合金具有一定的钝化能力,钝化区间比较宽广;在镍基合金CMSX-4表面上形成的腐蚀产物可大致分为两层,表层主要由Ni （OH）₂、Cr （OH）₃、Co （OH）₂和Al （OH）₃等氢氧化物组成,内层主要分布着NiO、Al₂O₃、CoO、Cr₂O₃和CrO₃等氧化物及组成合金基体的各种金属;由Ni （OH）₂和Cr （OH）₃等氢氧化物组成的腐蚀产物膜外层能够在腐蚀介质和金属之间产生较好的屏蔽效果;构成腐蚀产物膜内层的NiO、Al₂O₃、Cr₂O₃和CrO₃等氧化物有利于产物膜内层与外层之间建立一定的空间电荷区,对稳定腐蚀产物内层有很大帮助。研究表明CMSX-4合金在海洋性环境中具有一定的耐蚀性能。     

Valance electron structure of carbide-diamond interface and catalytic mechanism for diamond synthesis under high-pressure and high-temperature

The metallic films surrounding a synthetic diamond formed under high-pressure and high-temperature (HPHT) in the presence of Fe-based and Ni-based catalysts were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM). It was showed that the carbide was the primary carbon source for the nucleation and growth of diamond. Based on the EET (empirical electron theory in solid and molecules) theory, the valence electron structure of interface between carbide (Fe₃C, Ni₃C, (Fe, Ni)₃C) and diamond was calculated using the bonding length difference (BLD) method. The boundary criterion of Thomas-Fermi-Dirac-Cheng (TFDC): “the electron density being equal on the contacting surfaces of atoms” was applied to analyze the valence structure of carbide-diamond interface. The result based on the calculation valance electron structure is in good accordance with the experimental result. This study is very helpful to reveal the catalytic mechanism of diamond nucleation and growth and design the new catalyst for diamond synthesis.     

Growth of graphite film over the tops of vertical carbon nanotubes using Ni/Ti/Si substrate

A substrate with Ni/Ti/Si structure was used to grow vertical carbon nanotubes (CNTs) with a graphite fihn over CNT tops by thermal chemical vapor deposition with CH₄ gas as carbon source. The carbon nanotubes and the substrate were characterized by a field emission scanning electron microscope for the morphologies, a transmission electron microscope for the microstructures, a Raman spectrograph for the ctystallinity, and an Auger electron spectrometer for the depth distribution of elements. The result shows that when the thickness ratio of Ni layer to Ti layer in substrate is about 1, a graphite film with relatively good quality can be formed on the CNT tops.     

Correlation between structure and hardness of magnetron sputtering deposited CNx films

Carbon nitride films are deposited on Si (001) substrates by reactive dc magnetron sputtering graphite in a pure N2 discharge. The structure of carbon nitride films has been probed using Fourier transformation infrared, near edge X-ray absorption fine structure (NEXAFS) and high resolution electron microscopy (HREM), and the hardness has been evaluated in nanoin-dentation experiments. FTIR spectra show that N atoms are bound to sp1, sp2, and sp3 hybridized C atoms. C1s NEXAFS spectra show that the intensity of π* resonance is the lowest for the film grown at substrate temperature TS = 350℃, with a turbostratic-like structure and high hardness, while it is the highest for the film grown at TS = 100℃, with an amorphous structure and low hardness. The correlation between the structure and hardness of carbon nitride films has been discussed.     

Synthesis of nano onion-like fullerenes by using Fe/Al2O3 as catalyst by chemical vapor deposition

Nano-carbon materials were synthesized by the catalytic decomposition of acetylene at 400℃ by using Fe/Al₂O₃ as catalyst. The product was refluxed in 36% concentrated HCl at 60℃ for 48 h in order to remove the catalyst support. The samples were examined by scanning and high resolution transmission electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The results show that nano onion-like fullerenes encapsulating a Fe₃C core were obtained. These had a structure of stacked graphitic fragments, with diameters ranging from 15―50 nm. When the product was further heat- treated at 1100℃ for 2 h, nano onion-like fullerenes with a clear concentric graphitic layer structure were obtained. The growth mechanism of nano onion-like fullerenes encapsulating metal cores is suggested to follow a vapor-solid growth model.     

合金碳化物(Fe,Mo)_3C的磁性及磁致热力学性质

利用基于第一性原理的VASP软件计算钢中合金碳化物(Fe,Mo)_3C在0 K、0 Pa的磁矩和形成能,利用热力学平衡软件MTDATA计算合金碳化物(Fe,Mo)_3C的化学自由能改变量,利用Weiss分子场理论计算合金碳化物在12 T强磁场下的磁自由能改变量。结果表明,合金碳化物(Fe,Mo)_3C的磁矩主要来源于不同Wyckoff位置的Fe原子,8d位置的Fe原子对磁矩的影响比4c位置的Fe原子更大,而Mo原子会使合金碳化物的磁矩降低;合金碳化物Fe_2MoC、Mo_3C的形成能为负,表明这两种合金碳化物比Fe_3C和FeMo_2C更稳定;另外,Mo原子会降低合金碳化物(Fe,Mo)_3C化学自由能改变量,增大其磁自由能改变量。     

Fe-Ni-Cr玻封合金氧化膜及其封接性能

Ｎｉ４２Ｃｒ６Ｆｅ合金广泛用于制作显象管玻壳阳极帽。为了改善它作为软玻璃的气密性封接材料的性能，采用ＴＥＭ、ＸＲＤ、ＳＥＭ等技术研究此合金表面氧化膜的组成、结构及其气密性封接性能，以选择合适气密封接的氧化膜条件。试验结果表明，氧化初期以Ｃｒ２Ｏ３为主，后期以（Ｆｅ，Ｍｎ）Ｃｒ２Ｏ４为主。氧化膜表面为（Ｆｅ，Ｍｎ）Ｃｒ２Ｏ４，主要起浸润玻璃作用；氧化膜底层为Ｃｒ２Ｏ３，主要起致密稳定和与基体连接的作用。     

磁控溅射表面镀膜对Nd2Fe14B稀土永磁体抗腐蚀性能的影响

在Nd₂Fe₁₄B稀土永磁体基体表面,采用磁控溅射（直流+射频）技术制备了Ti/Ni,Ti/Al和Al/Ni等二元合金薄膜和Ti/Al/Ni三元合金薄膜。并通过中性盐雾试验、腐蚀失重计算、电化学腐蚀试验、金相观察等方式,对比研究了不同表面处理对Nd₂Fe₁₄B稀土永磁体基体抗腐蚀性能的影响,并构建了腐蚀模型。研究发现：Ti/Ni,Ti/Al和Al/Ni等二元合金薄膜和Ti/Al/Ni三元合金薄膜均有效地提高了Nd₂Fe₁₄B稀土永磁体基体耐中性盐雾腐蚀和电化学腐蚀的能力;Ti/Al/Ni三元合金薄膜较Ti/Ni,Ti/Al和Al/Ni等二元合金薄膜有更优良的综合耐腐蚀性能,其磁控溅射工艺参数为：Ar流量60 sccm,基片温度常温,Ni,Al,Ti的溅射功率都为250 W,基片转速20 r·min^-1,镀膜均速0.3 nm·s^-1,总计溅射时间1 h。     

γ′-（Fe1-xNix)4N薄膜结构及其磁学性能

采用直流磁控溅射方法, 在Si(100)单晶衬底上制备不同质量分数Ni掺杂的γ′-（Fe_1-xNi_x)₄N纳米晶薄膜样品,  并利用能谱分析、 X射线衍射(XRD)、 扫描电子显微镜(SEM)和振动样品磁强计(VSM)测试分析样品中Fe与Ni的原子比、 结构、 形貌及磁学性能. 结果表明, 在样品中掺杂Ni可提高材料的结构稳定性, 优化材料的软铁磁性能.