Sm_2Zr_2O_7-SiO_2复合材料的制备及介电性能研究

采用热压烧结的方法制备了Sm2Zr2O7-SiO2复合陶瓷材料,利用XRD、SEM、EDS等分析测试手段对复合材料的相结构、微观组织和成分进行了研究,测试了复合材料的介电性能,并对影响复合材料介电性能的机制进行了初步的探索。结果表明,Sm2Zr2O7与SiO2间发生反应生成Sm2Si2O7反应层,Sm2Si2O7具有较高的介电常数,随着SiO2含量的升高,Sm2Zr2O7-SiO2复合陶瓷材料的介电常数出现升高的趋势。     

碳纳米管增韧Sm_2Zr_2O_7基热障涂层复合材料的制备

本文提纯和分散了碳纳米管,采用共沉淀法制备出Sm2Zr2O7-CNT复合材料粉末,并用热压法制备出复合材料块体试样。研究了碳纳米管对Sm2Zr2O7微观形貌、相结构以及断裂韧性的影响。结果表明:在所得的复合材料中,碳纳米管均匀分散在Sm2Zr2O7基体中;复合材料的断裂韧性高于纯Sm2Zr2O7试样,并且随着碳纳米管含量的增多,复合材料强度和韧性有所提高,可以用界面结合强度及纤维拔出、纤维与基体的脱粘、纤维搭桥等理论来分析碳纳米管增韧复合材料的机制。     

La2(Zr0.7Ce0.3)2O7纳米粉体的制备与表征

采用化学沉淀法制备了高性能热障涂层用La2(Zr0.7Ce0.3)2O7陶瓷粉体.通过TG-DSC、XRD、SEM及TEM对前驱体的烧结温度、粉体物相及微观结构进行了分析.结果表明:制备的粉体为纳米级,且颗粒分布均匀,粒径大约30 ～ 50 nm;La2(Zr0.7Ce0.3)2O7是由烧绿石结构的La2Zr2O7固溶体和萤石结构的La2Ce2O7固溶体复合组成.     

稀土离子对0.6Ca0.6La0.267TiO3-0.4Ca(Mg1/3Nb2/3)O3陶瓷微观组织结构及微波介电性能的影响

采用固相合成方法制备钙钛矿结构的0.6Ca06La0.267TiO3-0.4Ca(Mg1/3Nb2/3)O3微波介质陶瓷,研究了La3+、Nd3+、Sm3+、Ce4+掺杂对0.6CLT-0.4CMN体系微观组织结构和介电性能的影响.研究结果表明:稀土离子的掺杂,在0.6CLT-0.4CMN体系优良介电性能基础上有积极的改善效果,不同程度稀土离子掺杂对该体系的晶粒尺寸、气孔率等微观组织结构也有不同的影响.La3+、Nd3+、Sm3+、Ce4+6掺杂完全固溶到0.6CLT-0.4CMN陶瓷相中,并没有改变陶瓷主晶相,但会在一定程度上发生晶面衍射峰偏移.适量掺杂Ln3可以有效促进0.6CLT-0.4CMN陶瓷的致密化,提高0.6CLT-0.4CMN体系陶瓷的微波介电性能.La3+、Nd3+、Sm3+、Ce4+掺杂可以有效提高Q ×f值,并在一定程度上降低谐振频率温度系数.其中,掺杂0.75mol; Nd3+的0.6CLT-0.4CMN体系微波介电性能最佳(εr=66.7,Q×f=13037 GHz,rf=22.59 ppm/℃)     

La2O3对莫来石陶瓷微观组织结构的影响

采共沉淀法制备了高纯度莫来石前驱粉体,掺杂La2O3制备莫来石复合陶瓷.利用XRD、SEM等方法对矿物组成和显微结构进行分析表征,并用X'pert High score Plus软件计算莫来石晶格常数,间接分析La2O3掺杂机理.实验结果表明,La2O3的掺杂改变了莫来石陶瓷的微观组织结构,莫来石晶粒由短棒状转变为网状和层状结构;La2O3的掺杂改变了物相组成,生成La1.66Al23.08O37.04,有助于提高莫来石陶瓷的致密性,在1500℃烧成时试样达到理论密度的95;.     

La_2Zr_2O_7∶Eu发光材料的共沉淀法制备与表征

采用共沉淀法制备La2Zr2O7∶Eu纳米粉体。采用热分析和XRD研究了前驱沉淀物在不同热处理温度下的物相组成。采用SEM观察所制备纳米粉体的显微形貌。使用荧光光谱仪测试了样品的激发光谱和发射光谱。结果表明,1200℃热处理2 h制备的La2Zr2O7∶Eu纳米粉体颗粒基本上呈球状,分散性较好,粒径分布在30~50 nm。光谱分析表明,La2Zr2O7∶Eu纳米粉体的激发光谱属于Eu3+的特征谱带,其中强度最大的峰值位于285 nm的谱带,属于O2--Eu3+的电荷迁移带。样品的发射光谱分布于570~650 nm之间,主发射峰位于585 nm。Eu3+的最佳掺杂量为5 mol%。     

高浓度Sm_2O_3掺杂的BIT陶瓷微结构与电性能研究

采用固相烧结工艺制备了高浓度Sm2O3掺杂的Bi4Ti3O12(BIT)基陶瓷材料。研究了不同的Sm2O3掺杂浓度和温度对BIT基陶瓷材料的显微结构及电性能的影响。结果表明:当Sm2O3浓度为12.0 mol%时,有Bi0.56Sm1.44Ti2O7第二相出现,BIT陶瓷室温介电常数为114,室温介质损耗(tanδ)为0.002;当Sm2O3浓度为6.0mol%时,陶瓷材料的室温介电常数为119,室温介质损耗(tanδ)为0.0027。     

Hf微量掺杂Sm2Ce2O7固溶体制备及热物理性能

采用高温固相烧结法制备了Sm2(Ge1-xHfx)2O7(x=0,0.025,0.05,0.075,0.1)固溶体,并对其相组成、显微组织及热物理性能进行了分析.结果表明,所合成的固溶体具有单一的萤石结构,其相对致密度均在90;以上.Hf掺杂增强了声子的散射程度,从而使其热导率与Sm2Ce2O7相比明显降低.Hf较小的离子半径使得其热膨胀系数随HfO2掺杂量增加而降低,但仍然满足热障涂层的要求.     

La2O3掺杂对BaTiO3-Nb2O5-Fe2O3陶瓷的晶体结构和介电性能的影响

研究了La2O3 掺杂对BaTiO3-Nb2O5-Fe2O3(BTNF)基陶瓷的晶体结构和介电性能的影响.XRD分析表明:La2O3掺杂陶瓷的(200)和(002)晶面衍射峰都发生了明显分裂,说明陶瓷均以四方相为主晶相.随着La2O3含量的增加,四方率先增大后减小.用SEM研究La2O3对BTNF基陶瓷微观结构的影响,结果表明:随着La2O3掺杂量的增加,试样的晶粒明显变小,La2O3显著的抑制了晶粒的生长.当La2O3掺杂量为0.15 mol;时,陶瓷晶粒生长比较均匀.陶瓷的室温介电常数大体上呈现出先增大后减小的趋势,当La2O3掺杂量为0.15 mol;时,有最大介电常数4562.     

La2O3对氧化镁陶瓷烧结性能与抗热震性能的影响

本文以纳米氧化镁为主要原料,La2O3为添加剂,聚乙烯醇为结合剂,制备烧结性能良好和抗热震性能优异的氧化镁陶瓷.通过常温力学性能、抗热震性能、XRD和SEM等手段对试样进行分析和表征,重点研究La2O3对氧化镁陶瓷烧结性能及抗热震性能的影响.结果表明:La2O3的加入能够促进氧化镁陶瓷的烧结.从微观结构看出La2 O3加入后可与氧化镁形成固溶体及一些不定形态物质,均匀分布在晶界处,减缓试样在热震时裂纹的尖端应力,阻碍裂纹延伸,有效提高氧化镁陶瓷的抗热震稳定性.经1640℃烧结La2O3的加入量为1;的试样相对密度最高,为99.72;;热震后经1560℃烧结La2O3的加入量为2;的试样常温耐压强度达到最大值,58 MPa.     

(Sm0.5Gd0.2Nd0.3)2(Hf0.3Ce0.7)2O7复合氧化物的热物理性能

为寻求新型热障涂层用陶瓷材料,本文采用高温固相烧结法制备了(Sm_0.5Gd_0.2Nd_0.3)₂(Hf_0.3Ce_0.7)₂O₇复合氧化物。利用XRD分析了其晶体结构,SEM分析其显微组织,膨胀仪测试其热膨胀性能,激光热导仪测试其热扩散系数。结果表明,成功制备了具有单一萤石晶体结构的(Sm_0.5Gd_0.2Nd_0.3)₂(Hf_0.3Ce_0.7)₂O₇复合氧化物。其显微组织结构致密,晶界清晰无其他相存在。由于复杂的元素组成和较大的原子量,其热导率明显低于7YSZ和Sm₂Ce₂O₇。其较低的热膨胀系数则归因于B位离子较小的离子半径,但其热膨胀系数依然满足热障涂层的要求。     

激光快速烧结合成A(WO4)2(A=Zr2+,Hf2+)的特性研究

利用二氧化碳激光快速凝固技术合成了负热膨胀材料ZrW2O8和HfW2 O8,Raman光谱和X射线衍射分析表明激光烧结合成的ZrW2 O8为正交相,压应力的大小估计在0.4～0.5 GPa之间,激光烧结合成的HfW2 O8,主要为立方晶系,含有极少量的正交系,压应力的大小估计在0.6 GPa左右,这是由于样品在快速凝固的过程中受到了压应力造成的.由于压应力的影响,二氧化碳激光快速凝固技术更适合HfW2O8的制备和合成.     

孔道结构钒铝磷酸盐(NH3CH2CH2NH2)[(VO)Al(PO4)2]的水热合成及热稳定性

用XRD,TG-DTA,FT-IR和SEM对水热法合成的孔道结构钒铝磷酸盐(NH3CH2CH2NH2)[(VO)Al(PO4)2]进行了热性能表征.该化合物中有机组份的分解温度,在氧化气氛中为305～529℃,在惰性气氛中为411～593℃.有机组分的分解逸出导致了结构的破坏,但晶体的微形貌没有发生明显的变化;温度继续升高,发生相变.该化合物热稳定性较其它含有机模板的孔道结构钒磷酸盐要高,主要原因在于结构中存在[AlO4]和[PO4]共顶连接而成的一维链,这种链增加了骨架的强度.     

Thermal conductivity of Tb2(MoO4)3 crystals at low temperatures

Thermal conductivity of the improper ferroic Tb₂(MoO₄)₃ was measured in the range 0.3 K–100 K by the method of the stationary heat flow. An additional maximum in thermal conductivity observed at 0.45 K is due to the anomaly of specific heat corresponding to the antiferromagnetic phase transition. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Growth,Thermal and Linear Optical Properties of the Non‐Centrosymmetric Hydrated Tetraborates Na2[B4O5(OH)4] . 3H2O (Tincalconite) and K2[B4O5(OH)4] . 2H2O

Large single crystals of the non‐centrosymmetric hydrated tetraborates Na₂[B₄O₅(OH)₄] . 3H₂O (Tincalconite) (point group 32) and K₂[B₄O₅(OH)₄] . 2H₂O(point group 222) were grown from aqueous solutions and the linear optical properties (refractive indices between 365 nm and 1530 nm and unpolarized absorption spectra) as a basis for nonlinear optical investigations were determined. The uniaxial positive sodium salt is not phase matchable; in the orthorhombic potassium compound type I phase matching is possible in the near infrared region. Thermal investigations indicate a phase transition at ≈285 K for Na₂[B₄O₅(OH)₄] . 3H₂O.     

Thermal expansion and structural properties of (CuAlTe2)1–x(CuAlSe2)x solid solutions

Investigations of the thermal expansion of (CuAlTe₂)_1–x(CuAlSe₂)_x solid solutions in the temperature range from 100 to 800 K have been carried out for the first time. It has been demonstrated that the thermal expansion coefficient α_L grows considerably in the temperature range from 100 to 300 K, whereas the temperature dependence above 300 K is rather weak. The isotherms of composition dependence of the thermal expansion coefficient α_L for 100, 293, 500 and 800 K were constructed, and it was found that linear relations could express them. The Debye temperatures θ_D , the average mean‐square dynamic displacements , the average root‐mean‐square amplitudes of thermal vibration RMS , the anion position parameter u using S. C. Abrahams & J. L. Bernstein (u_AB ) and J. E. Jaffe & A. Zunger (u_JZ ) models were calculated. The composition dependence of microhardness H using the phenomenological theory was also calculated, and it was discovered that this dependence has a non‐linear character with a maximum of 383 kg/mm² at x=0.67. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Physicochemical properties of the organometallic nonlinear optical crystal: MnHg(SCN)4(C3H8O2)

The growth morphology of MMTG (manganese mercury thiocyanate glycol monomethyl ether, MnHg(SCN)₄(C₃H₈O₂)) crystal was indexed according to the X‐ray powder diffraction spectroscopy. The density and Mohs hardness were determined at room temperature. The specific heat of the crystal is 458.6 J.mol^‐1K^‐1 at 300 K. The thermal expansion coefficient (TEC) along the a, b and c axis is a₁=6.89 × 10^‐5 K^‐1, a₂=6.78 × 10^‐5 K^‐1 and a₃=2.08 × 10^‐5 K^‐1, respectively. The sameness and difference of the TECs are interpreted on the basis of crystal structure. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Thermal induced structural properties of silver(I) sulphate (Ag2SO4)

The crystal structures of silver(I) sulphate, Ag₂SO₄, have been investigated as a function of temperature. A main feature is the phase transition from the low‐temperature ordered phase, F ddd, to the high‐temperature disordered phase, . In particular, the high‐temperature structure is solved from single crystal synchrotron X‐ray measurements. In this phase the title compound undergoes a colossal (anisotropic) thermal expansion of . This is presumably owing to a high anisotropic vibration state of one of the two crystallographically independent Ag‐atoms. Simultaneously occurring high ionic conductivity may be associated with silver ions moving along the ‐axis using a “paddle‐wheel” assisted percolative mechanism. Onset of metallic silver in the single crystals is documented, seemingly dependent on thermal pre‐history, mosaic structure and chemical synthesis. Possible mechanisms explaining this effect, comprising disproportionation or photo‐decomposition, are suggested.     

Crystallization of AgGaS2 melts enriched with Ag2S and Ga2S3

In this work we consider experiments with directed crystallization of melts with slight deviation from stoichiometric composition of AgGaS₂. The evolution of melt composition was calculated for both experiments using measured chemical composition of the solid phase. Also the difference in unit cell parameters and luminescence spectra for AgGaS₂ grown from the melts was found. Both monocrystal samples and samples synthesized from elementary Ag, Ga and S were used for thermal analyses. Obtained data suggests that different ways of preparing the samples are responsible for defects concentration and thus for so wide range (70°C) of melting temperatures reported in scientific literature. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Nonlinear optical properties of strontium tartrato‐antimonate(III) dihydrate,Sr[Sb2{(+)‐C4H2O6}2]·2H2O

The tensor of nonlinear optical susceptibility for second harmonic generation [d^SHG _ijk ] of hexagonal (point group 6) strontium tartrato‐antimonate(III) dihydrate, Sr[Sb₂{(+)‐C₄H₂O₆}₂]·2H₂O, was determined using the Maker fringes method and a Nd:YAG laser with a wavelength of 1064 nm. The largest component of the tensor d^SHG ₃₃₃ amounts two times d^SHG ₁₁₁ of α‐quartz. Effective nonlinear optical susceptibility d^SHG _eff is given for phase matching type I for several wavelengths (for type II d^SHG _eff is nearly zero). The thermal stability of crystals of Sr[Sb₂{(+)‐C₄H₂O₆}₂]·2H₂O was determined in the temperature range from 153 K to 573 K by means of thermal expansion measurements and thermogravimetry. The temperature dependence of thermal expansion coefficients is given in the range from 153 K to 293 K. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)