采用真空热压技术制备纳米金属钨块体材料

 采用真空热压技术,在570 ℃和1 GPa的条件下成功制备具有单相α-W结构、平均晶粒尺寸为34 nm、尺寸为Φ10 mm×1 mm的难熔金属钨纳米块体材料,其密度为理论密度的88.8%,显微硬度为4.8 GPa。纳米金属钨的密度和显微硬度随热压温度、热压压强和热压时间增大而升高。     

ZnO纳米块体材料的制备及其性能的研究

采用连续成型方式压制了纳米ZnO素坯，考察了素坯密度、烧结时间、致密化温度等参数与 成型方式的关系.用场发射扫描电镜表征了烧结体微观组织特征.测定了ZnO纳米块体材料中 硬度随烧结温度的变化规律.结果表明，采用连续成型方式可使素坯密度提高56％、烧结时 间缩短了3h、致密化温度降低200℃.场发射扫描电镜显示烧结体内部密度及颗粒尺寸分布 均匀.硬度测定结果显示ZnO纳米块体材料中显微硬度随烧结温度的变化不是单调的，而是随 烧结温度的升高显微硬度先升高后降低，拐点对应的晶粒尺寸为50—60nm. 关键词： ZnO纳米块体 连续成型 硬度     

高温高压烧结高硬度高致密度块体金属钨及钨基合金W-TiC

采用高温高压烧结方法,烧结纯钨和TiC颗粒弥散增强W-TiC合金材料,对钨及W-TiC合金的烧结致密化行为和力学性能进行了研究。结果表明:在压力为5.0GPa、温度为1 500℃的条件下烧结15min可获得良好的烧结样品,块体钨的致密度达到99.3%,硬度达到6.43GPa;在相同的高温高压烧结条件下,添加质量分数为1.5%的TiC,获得的W-TiC合金致密度达到99.0%,硬度达到7.58GPa。极端高压环境不但能抑制钨及钨合金在烧结过程中的晶粒长大,还能降低烧结温度,提高烧结效率,增加烧结体的致密性。在此基础上进一步探索了钨及钨基合金W-TiC的高压烧结动力学、微观结构、机械性能与烧结压力和烧结温度的关系。     

基片温度对SiNx薄膜结晶状态及机械性能的影响

利用微波电子回旋共振增强磁控反应溅射法在不同基片温度下制备无氢SiNx薄膜.通过傅里叶变换红外光谱、透射电子显微镜、台阶仪、纳米硬度仪等表征技术,研究了基片温度对SiNx薄膜结晶状态、晶粒尺寸、晶体取向等结晶性能以及薄膜的生长速率、硬度等机械性能的影响,并探讨了薄膜结晶性能与机械性能之间的关系.研究结果表明,在基片温度低于300℃时制备的SiNx薄膜以非晶状态存在,硬度值仅为18 GPa左右;基片温度在320-620℃范围内,SiNx薄膜中出现纳米晶粒,且晶粒尺寸随沉积温度的增加而增加,在沉积温度为620℃时达到最大,为20±1.5 nm;当沉积温度为700℃时,SiN<,x>薄膜的晶粒尺寸突然减小,但由于此时晶粒密度为最大,因此薄膜硬度达到最大值(36.7 GPa).     

氧化锌纳米晶高压下的晶粒演化和性能

用GS-1B型六面顶压机研究了ZnO纳米晶高压下的晶粒演化和性能，用X射线衍射仪和场发射扫描电子显微镜对高压样品的晶粒尺寸、微观形貌进行了表征.结果表明，高压下ZnO纳米晶存在压致晶粒碎化效应.硬度和伏安特性实验表明，高压调制后样品的显微硬度约是常压烧结样品硬度的2.3倍，非线性伏安特性明显优于常压烧结样品. 关键词： 氧化锌纳米晶 高压 压致碎化 非线性伏安特性     

基于纳米压痕法的多孔硅硬度及杨氏模量与微观结构关系研究

采用电化学腐蚀制备多孔硅，利用场致发射扫描式电子显微镜(field emission scanning electron microscope，FESEM)观测多孔硅的二维微观形貌，利用Nano Indenter XP中的纳米轮廓扫描仪组件(nano profilometry, NP)得到其三维拓扑分析图像，分析了微观结构差异的原因并讨论了多孔硅内部微观结构对其机械性能的影响；利用MTS Nano Indenter XP纳米压入测量仪器，研究了多孔硅的显微硬度和杨氏模量随压入深度的变化规律，比较了不同孔隙率多孔硅的机械性能差别.实验结果测得40mA/cm²，60mA/cm²，80mA/cm²和100mA/cm²四个不同腐蚀电流密度条件下制备多孔硅样品的孔隙率在60%—80%范围内，孔隙率随着腐蚀电流密度的增加而增大；在氢氟酸(HF)浓度为20%的条件下制备出多孔硅样品的厚度在40μm—50μm范围内；测得多孔硅的平均硬度、平均杨氏模量分别在0.478GPa—1.171GPa和10.912GPa—17.15GPa范围内，并且其数值随腐蚀电流密度的增加而减小，在纳米硬度范围内随压入深度的增加而减小，在显微硬度范围内其数值保持相对恒定，分析了样品表面、厚度、微观结构，及环境对其机械性能的影响，得到了多孔硅力学性能随其微观尺度形貌的变化规律. 关键词： 多孔硅 微观结构 硬度 杨氏模量     

烧结压力对碳化钽陶瓷维氏硬度的影响

为了探究烧结压力对不同晶粒尺寸碳化钽(TaC)力学性能的影响,通过高温高压技术对纳米、微米尺寸TaC粉末进行高温高压烧结,制备不同烧结条件下的块状TaC陶瓷。利用X射线衍射等表征方法对烧结样品的物相、元素分布、压痕形态进行表征,结果表明:TaC在烧结过程中物相稳定,且无杂质渗入。利用维氏硬度计对不同烧结压力(3.0、4.0和5.5 GPa)条件下的3种陶瓷样品进行维氏硬度测试,并进行微观结构分析,结果表明:随着烧结压力由3.0 GPa提升到5.5 GPa,微米尺寸TaC的维氏硬度(21.0 GPa)优于3.0、4.0 GPa下的纳米尺寸TaC维氏硬度(17.5、19.2 GPa)。此外,研究发现,测试维氏硬度时,3.0 kg应用载荷对测试TaC维氏硬度更加精确。研究结果对结构陶瓷烧结和超高温陶瓷硬度研究具有指导意义。     

B_6O/TiB_2复合材料的高温高压反应烧结

以B和TiO2为初始原料,依据压力可抑制原子长程扩散的动力学效应,通过高温高压(4~5GPa,1 200~1 500℃)一步反应烧结法制备B6O/TiB2复合材料。当B和TiO2物质的量之比为14.0∶0.8时,在5GPa、1 200℃、保温30min条件下得到的烧结样品性能较好,非晶硼(纯度93%~94%)过量混合粉末样品的硬度最高约为29GPa,高纯晶体硼(纯度99.99%)过量混合粉末样品的硬度最高约为32GPa,相对密度可高达99%。实验结果表明:高压抑制晶粒过度长大,同时又有利于B6O的合成,使其合成温度比常压下有所降低;在高压反应烧结过程中,合成的第二相TiB2晶粒和样品中的非晶相有效地消耗了残余应力,起到了增韧作用。     

铝纳米晶的正电子湮没研究

采用自悬浮定向流-真空热压法,在不同压强下制得铝纳米晶材料,并利用X射线衍射(XRD)和正电子湮没寿命谱(PALS)分析手段对铝纳米晶的结构和微观缺陷进行表征.XRD分析表明:所制备的铝纳米晶的晶粒度为48 nm.PALS分析表明:铝纳米晶的微观缺陷主要为类空位以及空位团,而微孔洞很少;短寿命τ1,中间寿命τ2以及其对应的强度I1,I2随压强变化而呈现阶段性变化;压制压强(P)低于0.39 GPa时制得的纳米晶空位团随压强的增加而逐渐转变为类空位;0.39 GPa P 0.72 GPa时,各类缺陷发生消除;P 0.72 GPa时,各类缺陷进一步发生消除.随压强的提高,铝纳米晶的密度增加,其显微硬度也明显增高.     

微米晶单斜氧化锆高压相变制备亚微米四方多晶氧化锆

高压相变已逐渐发展成为一种制备纳米/亚微米多晶陶瓷块体材料的有效方法。高压可以抑制原子的长程扩散进而抑制晶粒长大,高压下截获的新相不受初始材料晶粒尺寸的制约,通过热力学调控可以得到晶粒尺寸更小的多晶块体材料。陶瓷材料在特定热力学条件下通常会发生相变,新相的形成要经历形核、生长的过程。采用晶粒尺寸为2μm的单斜ZrO2与晶粒尺寸为50 nm的Y2O3以97:3的摩尔比混合,在5.5 GPa、800～1700℃温压区间内对初始材料进行烧结,采用X射线衍射、扫描电镜、透射电镜对所得样品进行表征。研究结果表明:高压下截获了单斜相和亚微米四方相复合的多晶ZrO2块体材料,1200、1400、1600和1700℃温度下获得的四方相的平均晶粒尺寸为(145±62) nm、(246±165) nm、(183±62) nm和(245±107) nm。利用高压相变以微米晶制备细晶粒多晶块体材料,可以避免常规方法中以纳米粉末为初始材料制备细晶粒多晶块体材料存在的团聚、吸附及晶粒长大的问题,进而发展一种以微米晶为初始材料通过高压相变制备高性能细晶粒多晶块体材料的方法。     

氧离子导体La1.9Y0.1Mo2O9细晶粒陶瓷的制备和电学性质研究

采用溶胶凝胶法合成的La_1.9Y_0.1Mo₂O₉纳米晶粉体, 结合微波烧结技术制备出不同晶粒度的La_1.9Y_0.1Mo₂O₉块体样品. 利用X射线衍射仪(XRD)、高分辨透射显微镜(HRTEM)、场扫描显微镜(SEM)对粉体及陶瓷块体的物相、 形貌进行了表征, 利用交流阻抗谱仪测试了样品不同温度下的电导率. 实验结果表明, 掺Y的La_1.9Y_0.1Mo₂O₉能将高温立方β 相稳定到室温; 块体样品致密均匀, 平均晶粒度范围在60 nm–4 μm之间; 致密度高的样品表现出高的电导率, 其中900 ℃烧结样品的电导率600 ℃时高达0.026 S/cm, 比固相反应法制备的La_1.9Y_0.1Mo₂O₉样品高出约1倍. 总结认为样品的致密性对电导率影响较大, 是通过影响晶界电导率来影响总电导率的, 样品的晶粒度(在60 nm–4 μm范围内)对电导率的影响还不能确定. 关键词： 氧离子导体 1.9Y_0.1Mo₂O₉')" href="#">La_1.9Y_0.1Mo₂O₉ 细晶粒陶瓷 微波烧结     

Effects of calcining temperature and heating rate on properties of high-permeability NiCuZn ferrites

The effects of calcining temperature and heating rate during sintering on densification and magnetic properties of high-permeability NiCuZn ferrites were investigated. It was confirmed that increasing calcining temperature lead to increase of the molding density (the pressed density of samples that have not been sintered), both molding density and activity of the calcined powders determined the sintering density (the density of samples after sintering) of the samples. With the calcining temperature of 1060 °C, the sintering density reached a peak. The initial permeability also peaked with the calcining temperature of 1060 °C, which could be attributed to the highest sintering density and relatively big grain size. Quality factor peaked with the calcining temperature of 1020 °C, which could be attributed to the biggest grain size. Calcining temperature had no distinct connection with Curie temperature, and it had a slight effect on the saturation magnetism (B_s) due to varieties of the sintering density. Further studies showed that heating rate had a pronounced effect on initial permeability and quality factor, which could be attributed to a variety in the grain size. The critical heating rate value was 2 °C/min in order to obtain high-performance NiCuZn ferrites with both high initial permeability and high quality factor.     

影响纳米Cu固体材料性能的工艺参数研究

 采用正交试验方法，通过XRD，MHV2000型显微硬度计（数显）和基于浮力原理等测试手段研究了压制压力、保压时间、退火温度和退火时间对自悬浮定向流－冷压法制备纳米Cu固体材料性能（晶粒大小、密度及显微硬度）的影响。结果表明：对晶粒度而言，退火温度是显著性影响因素，同时表明纳米Cu固体具有较好的热稳定性；对密度而言，压制压力是显著性影响因素；对显微硬度而言，退火时间是显著性影响因素。     

Dielectric permittivity of nickel ferrites at microwave frequencies 1 MHz to 1.8 GHz

NiFe₂O₄ prepared via the sol–gel technique were pre-sintered at 900 °C and synthesized at different sintering temperatures from 1,000 °C to 1,200 °C at 100 °C intervals. The samples were characterized for microwave dielectric properties. These samples were measured using Agilent Impedance/Material Analyzer at frequencies 1 MHz to 1.8 GHz. Results showed a decrease in the dielectric constant and loss factor with frequency except at the turning point, around 150 MHz, where the loss factor showed a gradual increase. However, both the dielectric constant and loss factor increase with increasing sintering temperature. The grain size and density also increased with increasing sintering temperature, but the porosity and grain boundary density showed a decrease. This paper was presented at the International Conference on Solid State Science and Technology 2006, Kuala Terengganu, Malaysia, Sept. 4–6, 2006.     

Improvement of sintering,nonlinear electrical,and dielectric properties of ZnO-based varistors doped with TiO_2

The effects of TiO_2 on sintering and nonlinear electrical properties of(98.5-x)ZnO–0.5MnO_2–0.5Co_2O_3-0.5Bi_2O_(3–x)TiO_2(x = 0.3,0.5,0.7,0.9 mol%) ceramic varistors prepared by the ceramic technique are investigated in this work.The optimum sintering temperature of the prepared samples is deduced by determining the firing shrinkage and water absorption percentages.The optimum sintering temperature is found to be 1200℃,at which each of the samples shows a maximum firing shrinkage and minimum water absorption.Also minimum water absorption appears in a sample of x = 0.9 mol%.Higher sintering temperature and longer sintering time give rise to a reduction in bulk density due to the increased amount of porosity between the large grains of ZnO resulting from the rapid grain growth induced by the liquid phase sintering.The crystal size of ZnO decreases with increasing TiO_2 doping.The addition of TiO_2 improves the nonlinear coefficient and attains its maximum value at x = 0.7 mol% of TiO_2,further addition negatively affects it.A decrease in capacitance consequently in the dielectric constant is recorded with increasing the frequency in a range of 30 kHz–200 kHz.The temperature and composition dependences of the dielectric constant and AC conductivity are also studied.The increase of temperature raises the dielectric constant because it increases ionic response to the field at any particular frequency.     

Ni对Fe_3Si化合物硬度影响的微观组织结构和电子结构研究

采用实验和第一性原理方法,从微观组织结构、电子结构、力学常数和布局分析研究了Ni浓度和烧结温度对Fe_3Si化合物硬度的影响.结果表明Ni含量为3.125at.%时,化合物具有最小硬度值.进一步增加Ni浓度,其硬度增大,B/c44比值先增加后减小,而G/B比值先减小后增加.但当浓度超过6.25at.%后,不仅不能改善Fe_3Si脆性,反而使合金脆化程度加剧,说明适当添加Ni可韧化Fe_3Si化合物.烧结温度较低时,电子结构对Fe_3Si化合物硬度的影响占主导作用,随烧结温度的升高,先析出的晶粒迅速长大,Ni含量对化合物硬度的影响有所减弱,微观组织结构的影响大于电子结构.     

Strong visible PL from the nc-Si thin film by Ni silicide mediated crystallization

We studied the growth of nanocrystalline silicon (nc-Si) thin film exhibiting a strong room temperature photoluminescence (PL) at 1.81–2.003 eV. The amorphous silicon was crystallized by Ni silicide mediated crystallization (Ni SMC) and then Secco-etched to exhibit the PL. The PL peak energy and intensity increase with increasing the metal density on the a-Si because of the reduction in the grain size down to 2 nm. The photoluminescence energy and peak intensity depend strongly on the Secco etch time because the grain size is reduced by etching the grain boundaries.     

Effect of the sintering temperature of ceramic manganites La0.7Mn1.3O3 ± Δ on their grain sizes, magnetic and electrical properties

The effect of the sintering temperature from 1070 to 1670 K of ceramic samples of lanthanum manganite La_0.7Mn_1.3O₃ on their grain size, structure, magnetic and resistive properties has been studied. An increase in the sintering temperature to 1270 K is shown to lead to an insignificant increase in the grain size and an increase in the density, fraction of the ferromagnetic phase in a grain, and colossal magnetoresistance. The ceramics sintering at temperatures higher than 1470 K is found to sharply increase the grain size; simultaneously, the grain takes a layered structure. The grain growth at these temperatures is established to be accompanied by manganese precipitation at the grain boundaries and likely in the grain interior. The increase in the sintering temperature is accompanied by appearance of a magnetically phase heterogeneity and a decrease in the Curie temperature and magnitude of the colossal magnetoresistance effect.