烧结工艺对原位合成ZrO2/TiB2复合陶瓷材料的力学性能影响

以TiC和B4C为原料反应生成TiB2,原位合成了TiB2含量为20％的ZrO2/TiB2复合陶瓷材料.分析了烧结工艺中烧结温度、保温时间和烧结压力对力学性能的影响.结果表明:当烧结温度由1650℃提高到1750℃时,复合陶瓷材料的抗弯强度由820 MPa增加到980 MPa,断裂韧性从7.2 MPa·m1/2提高到9.4 MPa·m12;当烧结温度升至1850℃时,抗弯强度和断裂韧性下降;显微硬度随烧结温度的升高而提高.在烧结温度1750℃压力为30MPa保温时间由30 min提高到45 min时,断裂韧性从8.6 MPa·m1/2提高到9.4 MPa·m1/2;保温时间增加至60 min时,断裂韧性下降;保温时间的变化对材料的抗弯强度、硬度影响不大.烧结压力对复合陶瓷材料的力学性能的影响较小.当烧结参数为1750℃、45 min、30MPa,ZrO2/TiB2复合陶瓷材料的抗弯强度、显微硬度、断裂韧性分别达到980 MPa、13.6 GPa、9.4 MPa·m1/2.     

Al2O3/TiB2/AlN/TiN复合陶瓷材料的力学性能及显微结构

将金属Al、Al3Ti和TiB2以AlTiB中间合金的形式引入Al2O3基体材料中,采用热压原位反应生成法制备了Al2O3/TiB2/AlN/TiN复合陶瓷材料.复合材料在烧结过程处于过渡液相烧结,并有新相AlN和TiN生成;对热压烧结后材料的硬度、断裂韧性和抗弯强度进行了测试和分析;分析了复合材料力学性能随AlTiB体积百分含量的变化规律;探讨了复合材料断面断裂方式的变化对其力学性能的影响;并对AlTiB中间合金的细化特性进行了分析.     

Gd2Ti2O7/ZrO2（3Y）陶瓷制备及力学性能研究

用共沉淀法合成Gd2Ti2O7纳米粉体,经真空烧结制备不同ZrO2(3Y)含量的Gd2Ti2O7/ZrO2(3Y)陶瓷。用XRD、SEM和力学性能试验等测试手段研究样品的物相、形貌和力学性能。结果表明:Gd2Ti2O7/ZrO2(3Y)陶瓷的力学性能随ZrO2(3Y)含量增加显著提高,ZrO2(3Y)含量为90vol%时,样品的维氏硬度、抗弯强度和断裂韧性最大值分别达到20.95GPa、199.21MPa和8.17MPa·m1/2。其原因是ZrO2(3Y)固溶导致晶粒尺寸减小,过饱和析出ZrO2(3Y)的颗粒弥散增韧,以及ZrO2(3Y)应力诱导相变增韧作用。     

以Ni/Al为助剂的TiB2-B4C陶瓷刀具制备及其切削钛合金性能研究

以Ni/Al为助剂在1800℃热压烧结制备了Ni/Al含量分别为0vol;(TB)、5vol;(TBNA5)和10vol;(TBNA10)的TiB2-B4C刀具材料,研究了其致密化机理、显微结构、力学性能和切削削钛合金(Ti6Al4V)的性能.结果表明,5vol;Ni/Al助剂的引入将TiB2-B4 C的相对密度从80;提高到96;,所制备的TBNA5刀具的抗弯强度、断裂韧性和维氏硬度分别为711 MPa、4.6 MPa·m1/2和22.7 GPa,Ni/Al助剂的引入显著改善了TiB2-B4 C陶瓷的致密化和抗弯强度,但是进一步增加Ni/Al助剂的含量(10vol;),将降低其抗弯强度和硬度.切削性能研究表明,与硬质合金刀具相比,TiB2-B4 C陶瓷刀具切削Ti6Al4V的初期磨损较快,但由于更好的高温性能,其后期磨损更慢,且磨损速率更加稳定,其主要磨损机理为粘结磨损和微崩刃,其中含5vol;Ni/Al助剂的TiB2-B4 C陶瓷刀具有相对较好的切削性能.     

TiB2/WC/h-BN纳微米复合梯度自润滑陶瓷材料的设计与制备

以纳米TiB2和微米TiB2为基体,WC为增强相,h-BN为固体润滑剂,采用热压工艺制备了TiB2/WC/h-BN纳微米复合梯度自润滑陶瓷材料,并测量了其力学性能.结果表明:与均质TiB2/WC/h-BN微米自润滑陶瓷材料相比,其抗弯强度、断裂韧性与硬度分别提高了15.8;、6.7;和11.1;.用压痕法测量得到材料内部的残余应力,其应力值呈明显的阶梯变化趋势,且关于中间层对称分布,材料表层存在残余压应力,可有效提高材料力学性能与使用性能.显微结构观察显示,TiB2/WC/h-BN纳微米复合梯度自润滑陶瓷材料晶粒细小、均匀,纳米TiB2颗粒分布均匀,材料断裂模式为典型的穿晶/沿晶混合断裂模式.     

水基流延成型和热压烧结制备碳化硼陶瓷及性能研究

以工业碳化硼粉末为原料、采用Si3N4磨球磨损法引入Si3N4烧结助剂,采用水基流延成型和热压烧结方法制备了碳化硼陶瓷.研究了氧含量、分散剂、pH值等因素对B4C陶瓷浆料分散性能的影响,采用XRD、SEM等对碳化硼陶瓷的物相、显微结构和第二相分布进行了表征,并测试了样品的维氏硬度、断裂韧性、抗弯强度和弹性模量.结果表明:经醇洗后的碳化硼粉末中氧化硼含量降低,有利于B4C陶瓷浆料的分散稳定.采用球磨磨损引入了Si3N4粉,在B4C基体中通过原位反应形成第二相SiC和BN,SiC和BN第二相颗粒在B4C基体中弥散分布均匀.在2100 ℃热压烧结样品的维氏硬度、抗弯强度、断裂韧性和弹性模量分别达到30.2 GPa、596.5 MPa、3.36 MPa·m1/2和362.3 GPa.     

热压烧结制备羟基磷灰石/透辉石陶瓷复合材料

采用热压烧结方法制备了羟基磷灰石/透辉石复相陶瓷材料,分析了羟基磷灰石基体与透辉石之间的界面结合、扩展及渗透过程,测试了复合材料的断裂韧性、硬度、抗弯强度与添加剂含量的对应关系,并对复相陶瓷材料的微观结构与力学性能进行了研究.结果表明:在1320℃,28MPa条件下热压烧结制备的复相陶瓷材料,其抗弯强度、断裂韧性均有明显提高,抗弯强度达到90MPa,断裂韧性达到1.07MPa·m1/2.     

感应区熔法制备Al2O3/MgAl2O4/ZrO2共晶陶瓷

利用感应区熔法制备了Al2O3/MgAl2O4/ZrO2共晶陶瓷.当坩埚壁温为2200℃、行走速度为2mm/h时,制备了φ10 mm ×62 mm表面光滑致密的陶瓷样品.扫描电镜微观组织图显示Al2O3相和MgAl2O4相为基体相,ZrO2相以棒状镶嵌在基体中.定向凝固共晶陶瓷硬度和断裂韧性达到12 GPa和6.1 MPa·m1/2,为预烧结体的2倍和1.7倍.气孔和晶界的消失及细小规整ZrO2相在基体中的弥散分布,有效提高了材料的硬度和断裂韧性.     

低温烧结3Y-TZP陶瓷的研究

以不同质量分数的MnO2-TiO2(质量比为1:1)为烧结助剂,在1300～1500 ℃下低温烧结制备了3Y-TZP陶瓷.对3Y-TZP陶瓷的相对密度、物相及显微结构、显微硬度、抗弯强度及断裂韧性进行了测试分析,并对烧结助剂的基本性能进行了表征.探究了烧结助剂及烧结温度对3Y-TZP陶瓷性能的影响.实验结果表明:在3Y-TZP陶瓷中加入烧结助剂MnO2-TiO2(质量比为1:1)可以实现低温烧结.试样的相对密度、显微硬度、抗弯强度、断裂韧性随烧结温度的升高先增大后降低.在烧结助剂为0.5wt;,烧结温度为1350 ℃时,试样的相对密度及力学性能都达到最大,在此条件下,试样的相对密度达97.16;,显微硬度为2032.8 HV,抗弯强度为300 MPa,断裂韧性为8.35 MPa· m1/2,且试样的断裂方式为晶粒拔出及晶粒断裂遵循着穿-沿晶断裂的模式,且晶粒极小.     

Ni-Al复合添加剂对超重力场燃烧合成TiB2基陶瓷组织性能的影响

通过在(B4C +Ti)体系中依次增加Ni-Al复合添加剂质量分数直至25;,采用超重力燃烧合成工艺,制备出系列TiB2基多相陶瓷.经XRD、FESEM、EDS分析,发现陶瓷基体由TiB2片晶、TiC晶粒及分布其间的NiAl合金相组成.增加Ni-Al复合添加剂质量分数直至15;,因促进陶瓷致密化、基体细化与组织均质化,增大TiB2基体相对陶瓷自增韧机制的贡献,故陶瓷相对密度、硬度、弯曲强度与断裂韧性均达到最大值,即分别为99.3; 、22.6±1.8GPa、948±52 MPa与13.6±1.1 MPa· m1/2.     

(C2N2H10)2Mg(HP2O7)2·2H2O synthesis and crystal structure

(C₂N₂H₁₀)₂Mg(HP₂O₇)₂·2H₂O, is a new inorganic organic hybrid structure. It has been synthetized using wet chemistry. Its crystal structure consists of cis- and trans-edge sharing [MgO₄(H₂O)₂] octahedra resulting in chains, which are linked via [HP₂O₇] units to form [Mg(HP₂O₇)₂(H₂O)₂]⁴⁻ layers. The Mg²⁺ cations and the ethylendiammonium cations are located on centers of inversion. The ethylendiammonium cations are alternately located in the interlayer space. The cohesion of the crystal is well ensured by coulombic interactions between anions and cations and by several hydrogen bonds. The diphosphate anion shows an eclipsed conformation.     

Crystal structure of Rb2[GeO2(OH)2]·2H2O

Single crystals of Rb₂[GeO₂(OH)₂] · 2H₂O are studied by X-ray diffraction. The crystals belong to the orthorhombic system, sp. gr. Pna2₁, a = 13.523(6) Å, b = 8.143(4) Å, c = 13.407(6) Å, Z = 8, R ₁ = 0.0506. In [GeO₂(OH)₂]^2? anions, the Ge-O distances (1.71–1.73(1) Å) are shorter than the Ge-OH distances (1.76–1.80(1) Å). Anions are linked to each other by pairs of hydrogen bonds to form infinite chains. The chains are linked by hydrogen bonds involving water molecules to form a 3D structure. The assignment of the bands in the IR spectrum of the compound under study is performed.     

通过SiO2涂层改善BaSi2O2N2∶Eu2荧光粉的热性能

本文研究了SiO2涂层对BaSi2O2N2∶ Eu2蓝绿色荧光粉发光性能和热性能的影响.采用溶胶-凝胶法制备了SiO2包覆的BaSi2O2N2∶Eu2+蓝绿色荧光粉.实验结果表明,最佳镀膜量为6wt;,当镀膜量大于此值时,荧光粉亮度迅速降低.涂覆SiO2后,在150℃下BaSi2O2 N2∶Eu2荧光粉的热猝灭性能提高了2.4;,在500℃热降解后荧光粉的发光性能提高了15;.SiO2涂层显著提高了BaSi2O2N2∶Eu2+荧光粉的热稳定性.SiO2涂层的作用机理是在荧光粉表面和氧化气氛之间形成阻挡层,保护Eu2的发光中心在热加热过程中不被氧化.     

Optical properties of the germanate melilites Sr2MgGe2O7, Sr2ZnGe2O7 and Ba2ZnGe2O7

Refractive indices and their dispersion in the wavelength range from 365 nm to 2325 nm and transmission ranges of the tetragonal melilite‐type germanates Sr₂MgGe₂O₇, Sr₂ZnGe₂O₇ and Ba₂ZnGe₂O₇ were determined. The uniaxial positive crystals Sr₂MgGe₂O₇ and Ba₂ZnGe₂O₇ both offer the possibility for phase matched second harmonic generation, a detailed analysis of phase matching conditions is given. The refractive indices of Sr₂ZnGe₂O₇ show an isoindex (isotropic) point at 467 nm. The investigation was performed on Czochralski grown large single crystals. The crystal structure of all three germanates were determined by means of X ‐ray diffraction. The results corroborate unmodulated melilite‐type structures at room temperature. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate, [C6H5CH2CHCH2CH2NH2CH2CH2]2HPO4·5H2O

The salt bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate is orthorhombic with the following unit cell dimensions: a = 11.235(2) Å, b = 27.924(6) Å, c = 9.321(4) Å space group Pca2₁ with Z = 4. The structure was solved by the Patterson method and refined to final R value of 0.049 for 1802 independent reflections. The flack parameter is 0.14 with an e.s.d. of 0.23. The structure consists of infinite parallel two-dimensional [110] planes built of mutually connected ions and water molecules by strong O—H,...,O and N—H,...,O hydrogen bonding. There are no contacts other than normal van der Waals interactions between the layers.     

Identification of a new family of diphosphate compounds, AI2BII3(P2O7)2: Structures of Ag2Co3(P2O7)2, Ag2Mn3(P2O7)2, and Na2Cd3(P2O7)2

Syntheses and single-crystal X-ray structural results are reported for three new mixed diphosphates of the family A^I ₂B^II ₃(P₂O₇)₂; Ag₂Co₃(P₂O₇)₂ (I), Ag₂Mn₃(P₂O₇)₂ (II), and Na₂Cd₃(P₂O₇)₂ (III). All crystallize in the triclinic system, space group P1 bar: (I) a = 5.351(4), b = 6.375(4), c = 16.532(4) Å, = 80.83(6) = 81.45(4), = 72.87(5)°, V = 528.9(6) ų, Z = 2, D _calc = 4.649 mg/m³, R/Rw = 0.0428/0.0548 for 3949 obs. reflns; (II) a = 5.432(7), b = 6.619(6), c = 16.51(3) Å, = 80.78(8) = 82.43(9), = 72.82(7)°, V = 557.7(13) ų, Z = 2, D _calc = 4.338 mg/m³, R/Rw = 0.0679/0.1303 for 2100 obs. reflns and (III) a = 5.67(3), b = 7.08(4), c = 7.90(4) Å, = 77.0(2), = 82.5(2), = 67.8(2)°, V = 286(3) ų, Z = 2, D _calc = 4.249 mg/m³, R/Rw = 0.0307/0.0342 for 1945 obs. reflns. (I) and (II) are isostructural but (III) is of a different type. All three structures are characterized by layers of P₂O₇ groups alternating with layers of mixed metal atoms. Differences are seen in the conglomerate bonding patterns of B atoms and in the irregular geometry of Ag in (I) and (II) compared to the octahedral bonding seen for Na in (III). The differences in structure may be understood in terms of the ratios of the ionic radii of A and B atoms.     

Synthesis and characterization of (NH4)2CuBr2Cl2·2H2O crystals

Single crystals of a new compound, (NH₄)₂CuBr₂Cl₂.2H₂O, were grown from saturated aqueous solution at room temperature by slow evaporation method. The grown crystals were characterized through elemental, powder XRD, thermal and DSC analyses and FTIR and far IR spectra. The elemental analysis and the decomposition pattern formulated using the TG‐DTG studies confirm the stoichiometry of the compound. The crystallinity of the compound is confirmed from the powder XRD pattern. A preliminary single crystal X‐ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with a = 7.7466 Å, b = 7.783 Å and c = 8.1211 Å. The low temperature DSC shows thermal anomalies at –161.1, –156.5, –152.4, –145.2, –134, –18.5, and 1.4°C during the heating run and at –4.3, –54.8, –66.1, –90.6, –109.7 and –147.2 °C during the cooling run. The thermal hysterses indicate first order phase transitions in the title compound at these temperatures. The FTIR spectra were used to assign the characteristic vibrational frequencies due to NH₄⁺, CuX₄^2– ions and other chemical bonds. The effect of substitution of two bromine atoms on the phase transitions of a closely related crystal, diammonium tetrachloro cuprate dihydrate is also discussed. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Oxygen-conducting compounds with La2Mo2O9 structure in the ternary system La2Mo2O9-Sm2W2O9-Sm2Mo2O 9 + : Synthesis and properties

Polycrystalline samples in the ternary system La₂Mo₂O₉-Sm₂W₂O₉-Sm₂Mo₂O ₉ ⁺ were synthesized in air. The region of the existence of compounds with the lanthanum molybdate (La₂Mo₂O₉) structure in this system was determined. The polymorphism of the synthesized compounds was studied. Doping with samarium or with samarium and tungsten was shown to lead to the suppression of the transition between the monoclinic and cubic phases α → β and the appearance of the transition β _ms → β between two cubic phases. In samples with a high samarium content, the phase transition β _ms → β manifests itself as significant anomalies in the temperature dependences of the dielectric permeability and electric conductivity. An increase in the concentration of samarium in the samples leads to a substantial decrease in the conductivity compared with the nondoped compound La₂Mo₂O₉.     

Structure of {Pb[S2CN(C2H5)2]2(1,10-phenanthroline)}2

Lead (II) nitrate reacts with 1,10-phenanthroline and sodium diethyldithiocarbamate in water to produce yellow bisdiethyldithiocarbamata 1,10-phenanthroline lead(II). Crystals from water are triclinic, space group $P\bar 1$ (#2),a=10.53(2) Å,b=11.050(12)Å,c=24.74 (3) Å, α=94.71 (9)⁰, β=98.15(11)^o, γ=114.11(9)^o,V=2569(6) ų,Z=2. Each lead atom has approximate pentagonal pyramid coordination geometry through the nitrogens of a phenathroline and sulfurs of two dithiocarbamates. Additionally, complexes form loose dimers in which lead atoms are weakly coordinated to a sulfur in an adjacent complex. IR and proton nmr spectrum of the complex are consistent with the solid state structure.