烧结气氛对BiFeO3陶瓷性能影响的研究

采用微波水热法合成纯相的BiFeO3粉体,在不同气氛(N2和O2按不同比例混合)下烧结BiFeO3陶瓷。利用XRD、SEM、LCR等测试方法研究了不同的烧结气氛对BiFeO3陶瓷晶体结构、微观形貌及电性能的影响。研究结果表明:所制备的BiFeO3陶瓷均具有单一菱方相钙钛矿结构,BiFeO3陶瓷内部晶粒的显微形貌表现为紧密排列的圆形颗粒结构。样品的介电性能测试表明,介电性能随气氛中N2比例的增加而得到提高。当气氛中N2∶O2=9∶1时,介电常数和介电损耗值在5 kHz下分别为205和0.055,此时得到最优的介电性能。室温下的电滞回线测试结果表明在富氮气氛下烧结能提高样品的铁电极化值和击穿场强。     

钛(Ⅳ)固溶氧化镁纳米粉体的制备与表征

采用液相共沉淀方法,以Mg(NO3)2·6H2O和Ti(OC4H9)4为起始原料,NH3·H2O为沉淀剂,PEG为分散剂,冰乙酸为修饰剂,制备了钛(Ⅳ)固溶氧化镁纳米粉体.利用XRD,XPS和TEM等分析手段对粉体的物相组成、结构和形貌等进行了表征.结果表明Ti4+固溶到Mgo的品格中,物相只有立方晶系的方镁石结构Mgo相组成,无其它相存在.所制得的粉体颗粒尺寸小(约40～50 nm)、粒度分布均匀,具有良好的分散性能.     

BaCe_(1-x)Mn_xO_3材料的制备和电性能研究

采用高温固相法制备了BaCe1-xMnxO3-δ(x=0.05~0.30)。运用X射线衍射(XRD)和扫描电子显微镜(SEM)分别对BaCe1-xMnxO3-δ系列试样的物相结构和微观形貌进行了表征,并应用IM6e型电化学工作站测定了不同温度(250~800℃)下试样的交流阻抗谱。结果表明:x=0.05~0.10样品为钙钛矿型单相结构,x=0.10~0.30时样品中有第二相Ba2MnO3形成。在1500℃烧结的样品,随着Mn2+掺杂浓度的增大,试样的致密性有所提高,试样的电导率增大。当x=0.30时,BaCe0.7Mn0.3O3-δ试样在空气气氛800℃电导率达1.14×10-3S.cm-1。     

Bi4Si3O12-Bi4Ge3O12赝二元系统析晶行为及其晶体生长

本文采用固相合成方法制备了Bi4(GexSi1-x)3O12(BGSO)固溶体(x=0～0.4),研究了它的固溶特性和析晶行为。实验结果表明,不同组成混合料在900℃左右固相反应能生成BGSO纯相;XRD分析显示,在x=0～0.4区间内,Bi4Si3O12和Bi4Ge3O12可以完全互溶,其晶格常数随x的增加呈线性增长。采用坩埚下降法生长了x=0.15组成的BGSO混晶,获得了透明晶体,并测试了晶体的光学性能。     

放电等离子烧结制备Ba2+掺杂γ-La2S3陶瓷及其性能研究

以气固反应硫化制备的γ-La2S3粉体为原料,采用放电等离子烧结(SPS)技术制备出γ-La2S3多晶陶瓷.研究了Ba2+掺杂量对得到γ-La2S3粉体物相结构的影响,并分析了烧结温度、再硫化工艺参数对γ-La2S3多晶陶瓷微观组织结构和红外透过率的影响.结果表明:掺入Ba2有利于低温获得稳定的高温型γ-La2S3相,在nLa/nBa为5 ～15时能够得到纯相的γ-La2S3粉体.在烧结温度为1150℃,保温时间为5min时制备出的γ-La2S3陶瓷致密,无明显气孔,在CS2气氛下再硫化2.5h后,在10 ～ 14μm波段的红外峰值透过率达到42％.     

(1-4x)NBT-3xKBT-xBT系压电陶瓷电性能研究

采用传统固相法制备了(1-4x)NBT-3xKBT-xBT(x=0.020～0.035)体系压电陶瓷.采用XRD分析发现该体系陶瓷都能形成单一的钙钛矿型固溶体,并在0.025≤x≤0.032范围内具有三方和四方共存结构,为该体系的准同型相界.当x=0.028时,d33=162 pC/N,Qm=203.29,kp=0.234.电滞回线分析表明,(1-4x)NBT-3xKBT-xBT体系陶瓷随着KBT和BT含量的增加具有从铁电体向反铁电体转变的趋势.     

射频磁控溅射法制备TiO2-xNx薄膜的结构性能研究

利用射频磁控溅射法室温下在Si(100)衬底上制备了N掺杂的TiO2薄膜,并且采用x射线衍射(XRD)、X射线光电子能谱(XPS)和透射光谱对薄膜进行了表征.XRD结果表明在纯Ar和N2(33.3;)/Ar气氛下制备的TiO2-xNx薄膜均为单一的金红石相,薄膜结晶性良好,呈高度(211)择优取向,而在N2(50.0;)/Ar下制备的薄膜结晶性明显变差;对于N掺杂的TiO2薄膜,XPS表明部分N原子进入TiO2晶格,并且以N-Ti-O、N-O键以及间隙式N原子形式存在;透射光谱表明掺N后的TiO2薄膜吸收边发生了红移.     

原位反应烧结法制备MgAlON复合材料

实验原料选用高纯电熔镁砂(粒径3～1 mm);α-Al2O3(活性)微粉(粒径≤5μm);电熔镁铝尖晶石(粒径≤1mm);Al粉(粒径≤0.088 mm);化学纯MgO(粒径≤0.04 μ m)和少量的活性材料,氮化气氛下原位反应制备MgAlON复合材料,考察了氮化烧结后试样的常规性能、物相组成、显微结构.结果表明:1500℃下,氮化气氛中耐火基质料为Al-Al2O3-MgO系的混合粉可以通过原位反应制备MgAlON复合材料;骨料种类的不同,不影响MgAlON矿相的生成.且MgAl2O4-MgAlON材料的烧结性能及氮化效果较好,常温强度也较高.试样骨架结构是骨料大颗粒在烧结中形成的,骨架中填充着反应合成的MgAlON晶粒和骨料小颗粒,使得烧成后的试样内部结构致密;微晶结构以及晶须的存在有利于提高材料的常温力学性能.     

碳氮纳米晶体的制备与表征

采用机械球磨法,以石墨为反应前驱物,在充有300kPa压力的氨气气氛下连续球磨200h,然后在氨气气氛、650℃以上的温度条件下热处理4h,制备出C3N4纳米单晶.X射线粉末衍射(XRD)确定出样品中主要晶相为β-C3N4,此外还有少量的α-C3N4.电子衍射、红外光谱测试结果进一步表明产物的结构为C3N4单晶.     

Sn1-x-yMnxSbyO2体系固溶体的相关系及形成机制

本文采用化学共沉淀法制备一系列配比的三元 Sn1-x-yMnxSbyO2(y=0.05)固溶体,利用 XRD、TG-DTA 等分析了在 600～1000℃退火温度下的固溶体物相组成,并根据分析结果绘制了该固溶体在固相线下的相图,进而探讨了 Sn1-x-yMnxSbyO2(y=0.05)固溶体的形成机制.结果表明:在600～1000℃退火温度下,Sn0.9Mn0.05 Sb0.05O2 固溶体只存在四方金红石相的SnO2物相,锑和锰主要以Sb5+、Mn3+、Mn4+的形式进入SnO2晶格形成有限固溶体;Sn0.7Mn0.25Sb0.05O2 和 Sn0.6Mn0.35Sb0.05O2 固溶体在 700℃、800℃出现了立方相方铁锰矿型 Mn2O3,1000℃出现了四方相黑锰矿型 Mn3O4,Sn0.6Mn0.35Sb0.05O2 固溶体在1000℃时还出现Sb3+Sb5+O4 物相;固相线下 Sn1-x-yMnxSbyO2(y=0.05)固溶体相图包括六个区域,其中富含锡的(Sn,Mn,Sb)O2ss 区域是唯一的单相区,锰和锑主要分别以 Mn2O3 和Sb2O5 的形式溶入 SnO2 晶格中,并达到饱和.(Sn,Mn,Sb)O2ss 固溶体氧化物可作为良好导电性和耐腐蚀性的阳极中间层材料.     

Mn、Cu共掺ZnO磁性的研究

本文采用水热法,分别以ZnO、Zn(OH)2为前驱物,添加一定量的MnCl4.4H2O和CuSO4.2H2O, 3mol/LKOH作矿化剂,温度430℃,填充度35%,反应24h,制备了Mn、Cu共掺ZnO晶体。当前驱物为Zn(OH)2时,所得晶体大部分为短柱状晶体,显露正负极面{0001}、{0001-}、负锥面-p{101-1-}和柱面m{1-010},长度约为30 ～50μm。少部分晶体为单锥六棱柱状,显露正锥面p{101-1},柱面m{1-010},负极面-c{0001-},晶体的长度约为100μm,长径比为5:1。当ZnO用作前驱物时,短柱状晶体长度大约为10 ～30μm,晶体的六棱对称性都出现较大的偏差。X射线荧光能谱分析表明,前驱物为ZnO、Zn(OH)2时,Mn离子含量在分别为3.19%和1.62%原子分数,没有检测到Cu离子。虽然Mn、Cu离子的掺入会明显影响晶体形态,磁性测量显示掺杂Mn、Cu的ZnO仍为反铁磁。     

Physical properties of single crystalline CeNi4.2Mn0.8

A single crystal CeNi_4.2Mn_0.8 was grown by the Czochralski method from a levitating melt. The structural, magnetic, electrical transport and electronic structure properties were examined. X‐ray diffraction confirms the hexagonal structure. The f occupancy n_f and the coupling Δ between the f level and the conduction states are derived to be about 0.95 and 100 meV, respectively. The X‐ray photoemission spectroscopy shows that Ce ions in CeNi_4.2Mn_0.8 are in the intermediate valance state. The temperature dependence of resistivity exhibits the metallic character of this compound and reveals a small inflection at 136 K. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of nano ZnS doped with Mn

Nanocrystalline samples of Zn_1‐xMn_xS (x = 0.0, 0.02, 0.04) were synthesized by chemical precipitation method and characterized for magnetism. EPR studies showed an evidence of ferromagnetism around room temperature. Hysterisis from vibrating sample magnetometer supports the observation. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Electron Spin Resonance of Mn2+ in Hemimorphite

The Electron Spin Resonance of Mn²⁺ in natural crystals of hemimorphite was studied at RT, X-band. No fine structure other than the central M = | + 1/2 〉 ⇆ | −1/2 > transition with allowed (Δm = 0) and forbidden (Δm = ±1) hyperfine transitions were observed. The spectrum was fitted with the spin Hamiltonian parameters g = 2.001, A = −84.6 × 10⁻⁴ cm⁻¹. The crystal field parameter D was estimated equal to (8 ± 2) × 10⁻³ cm⁻¹. The most striking result is the size of the hyperfine splitting constant favoring occupancy of sixfold coordinated sites.     

On the bindings in the crystal phases of Mn

The heterotypism of Mn may be interpreted energetically when a temperature dependent valence electron concentration is supposed which takes on values between 2.2 and 0.6 electrons per atom. The room temperature phase Mn.r (= αMn) belongs to a series of structural types: Cr₃Si, U.h₁ (= βU), Mn.r, which occur in alloy systems such as MoRe_M (M = undetermined mole number) at certain values of the averaged group number (AGN) of the perodic system of chemical elements (rule of Raub). An interpretation of the series by means of the plural-correlations model becomes possible when instead of the (Ekmanian) AGN count another (non-Ekmanian) electron count is used. The phase Mo₃Re (Cr₃Si-type) yields a simple bonding type (binding) which undergoes moderate transformations to form the phases Mo₂Re₃(U.h₁) and MoRe₃(Mn.r) and the binding of MoRe₃ may be taken to be valid also for Mn.r; it corresponds to the valence electron concentration N′^A_b = 2.16. For the high temperature phases Mn.h₁ (= βMn) and Mn.h₂ (= γMn) the values N′^A_b = 1.6 and 1.0 are probable and allow the brass-like structures Mn.h₁ (C20) and Cu(Fl). The binding of Mn.h₂, incidentally, explains the occurrence of the tetragonal metastable phase Mn.m. finally Mn.h₃ (= δMn) crystallizing in the W-type is isodesmic to Fe.h₂ (= δFe), i.e. of the same binding.     

Interdiffusion of Mn in austenitic and ferritic CrNi steels

The interdiffusion coefficients of Mn have been obtained in different austenitic and ferritic CrNi-steels between 1000 and 1300 °C using Boltzmann-Matano and Grube methods. The diffusion coefficients of Mn (≦ 2 wt%) were found to be independent on its concentration. Small variations in Cr and Ni contents in both types of steels showed neglegible effect on manganese diffusion. The interdiffusion results in austenitic steels are comparable with the Mn tracer diffusion in Type 316 steel. The results of diffusion of manganese in ferritic CrNi steels reported here are first to be published.     

On the state of Mn impurity implanted in Si

The state of manganese impurity in implanted silicon at implantation doses of up to 5 × 10¹⁶ cm^?2 has been investigated by X-ray diffraction and transmission electron microscopy. It is established that, after short-term vacuum annealing at 850°C, most of the implanted manganese impurities are in microinclusions up to 20 nm in size formed by a tetragonal silicide phase of the Mn₁₅Si₂₆ type.     

Mn3O4纳米粒子的合成及表征

以 KMnO4和乙醇为原料,常压下50～60 ℃反应生成前驱物,将此前驱物转移至反应釜中,在190 ℃反应4 h,采用溶剂热法合成Mn3O4纳米粒子.探索了反应温度对产物结晶度及产物在水中分散性的影响.利用X射线衍射仪(XRD)、透射电子显微镜(TEM)、红外吸收光谱(IR)对产物进行表征.结果表明,反应温度为190 ℃时,产物Mn3O4纳米粒子的结晶度最大,在水中分散性最好,为四方晶系,平均粒径在50 nm左右.该方法的突出特点是Mn3O4纳米粒子的合成量大,反应时间短,效率高.     

水热法合成掺Mn橙色刚玉晶体

本文采用水热法,在430℃、40MPa的压力下合成出了纯α-Al2O3晶体.在同样的条件下,通过掺入Mn(NO3)2合成了掺Mn橙红色刚玉晶体.掺入Mn(NO3)2时,合成产物有两种晶体,一种是无色刚玉晶体,体积较小,为六棱柱状,直径30～40μm,高为30～40μm.另一种晶体为橙红色掺Mn刚玉晶体,其外形轮廓近乎球形,晶体表面有十分粗糙的生长阶梯,台阶高度为2～5μm,晶体高200～300μm,直径200～300μm.