锆酸镧的固相合成及其热障涂层的抗热震性能研究

用高温固相反应法合成了锆酸镧(La_2Zr_2O_7)陶瓷粉末,用大气等离子喷涂(APS)法制备了热障涂层。通过TG-DSC,XRD,Raman,FTIR和SEM等表征手段对合成的粉末进行结构和形貌分析,研究了煅烧温度和时间对La_2Zr_2O_7形成过程的影响以及固相合成粉末对涂层抗热震性能的影响。结果表明:高温固相反应法合成的La_2Zr_2O_7具有单一的烧绿石结构,相结构非常稳定,随着煅烧温度的升高,La_2Zr_2O_7相的含量和晶粒度均增加;在煅烧温度1400℃分别保温不同时间,La_2Zr_2O_7相的含量变化不明显,晶粒度随保温时间的延长而缓慢增加,二次煅烧粉末的相含量和晶粒度都大幅提高。La_2Zr_2O_7粉末所对应涂层的抗热震性能随粉末煅烧温度的升高而降低。     

聚苯硫醚的动态力学行为研究

本工作借助TBA技术研究了聚苯硫醚(PPS)的动态力学行为。结果表明,PPS的端基和分子量,热处理方式(固相处理或熔融处理)和处理时间,试样的热历史(淬火或退火)及制辫子所用的纤维的表面性质(玻璃纤维、碳纤维和石墨纤维及其表面处理)等因素对其动态力学行为均有影响。这些动态力学行为特征的变化与这些因素所引起的PPS的分子结构和超分子结构的变化有关。     

聚苯硫醚热交联特性研究进展

聚苯硫醚是一种具有典型交联特性的半结晶型热塑性聚合物,在不同气氛条件下进行热处理会发生不同程度的热交联、链增长、氧化交联和氧化反应,热处理后的PPS树脂分子量增加,热稳定性提高,结晶性能也会发生变化。主要围绕PPS树脂热交联处理的机理研究及其在工程上的应用,重点阐述了不同热处理条件对PPS树脂性能的影响及其与工程应用的结合。对PPS树脂后处理过程中存在的问题进行总结,提出了将热交联处理和增韧结合起来同步完成的研究思路。     

冷却速度对Mg-Gd-Y-Zr合金组织和固溶行为的影响

通过金相显微镜、扫描电镜、X射线衍射、差热(DTA)分析等手段,研究了砂型差压铸造和金属型Mg-10Gd-3Y-Zr合金的组织和固溶行为差异.结果表明,与金属型相比,砂铸Mg-10Gd-3Y-Zr合金的晶粒明显粗大,而第二相含量则相对较少;冷却速度不仅影响了合金的铸态组织,同时也影响了合金随后的固溶行为.金属型条件下,500℃× 8 h的热处理已使第二相达到完全固溶,而砂型铸造合金则需525℃×8 h的高温固溶才能使第二相溶解完全.     

热处理对非晶态合金Nd9(FeCoZrAl)85B6磁性能的影响

采用ＸＲＤ等方面研究了单辊急冷法制备的低钕含量的快液Ｎｄ９（ＦｅＣｏＺｒＡｌ）８５Ｂ６非晶态合金在不同热处理工艺下的相组成、晶粒尺寸大小及其磁性能变化规律。热处理工艺对Ｎｄ２Ｆｅ１４Ｂ相和μ－Ｆｅ相析出、晶凿尺寸大小和合金的磁性能具有明显影响。当热处理温度较低时Ｎｂ２Ｆｅ１４Ｂ相析出不充分,并出现不均匀长大,其晶粒尺寸反而较大;当热处理温度过高时,Ｎｄ２Ｆｅ１４Ｂ相虽然析出充分,但其晶粒尺寸也明显     

Nd-Fe-B磁体烧结过程晶粒长大行为的研究

定量描述了Nd-Fe-B磁体烧结过程晶粒长大行为，分析了烧结温度、烧结时间、合金粉末粒度及其分布对烧结过程晶粒长大的影响，讨论了烧结过程晶粒长大机制。在Nd-Fe-B磁体烧结过程开始之后的0—1h时间区段，晶粒长大迅速；随着烧结时间的延长，晶粒长大速度减小。合金粉末平均粒度增大，或者合金粉末粒度分布范围增宽，显著促进Nd-Fe-B磁体烧结过程中晶粒的长大。在Nd-Fe-B磁体的烧结过程中，存在两类晶粒长大机制，即Nd2Fe14B颗粒的溶解与析出、Nd2Fe14B颗粒的并合与长大。Nd2Fe14B颗粒的并合与长大不仅使磁体的平均晶粒尺寸增大，也使晶粒尺寸分布范围增宽，是烧结Nd-Fe-B磁体显微组织中出现异常大晶粒的根本原因。     

纳米晶掺钇硬质合金粉末的制备

采用高能球磨法制备了纳米晶掺Y硬质合金粉末。用XRD，SEM和DTA等分析检测手段，研究了纳米晶掺Y硬质合金粉末的结构、形貌和相的变化。结果表明：高能球磨45h，可获得晶粒尺寸约为8nm的掺Y硬质合金粉末；微量Y的加入，有利于硬质合金粉末晶粒的细化；在25～45h范围内，随着高能球磨时间的延长，粉末晶粒尺寸减小，且掺Y硬质合金粉末的晶粒尺寸比未掺Y的硬质合金粉末晶粒尺寸要细一倍；高能球磨25h，粉末中Co的X射线衍射峰消失。高能球磨掺Y硬质合金粉末的DTA曲线在626℃出现了1个尖锐的放热峰。高能球磨掺Y硬质合金粉末固结之后，其合金晶粒细小，机械性能较好。     

Gd5Si2Ge2相的线状缺陷

使用X射线粉末衍射(XRD)表征了电弧炉熔炼的Gd5Si2Ge2.2合金的相组成,结果表明Gd5Si2Ge2.2合金主要由Gd5Si2Ge2相和GdGe相构成。扫描电镜(SEM)分析表明,Gd5Si2Ge2晶粒内部有大量规则分布的线状特征;透射电镜(TEM)研究发现了Gd5Si2Ge2相的基体上存在两种不同形态的线条组织,选区电子衍射证明两种不同形态的线条组织既非第二相也非孪晶;根据高温原位金相观察的结果推测,该线状组织是在液-固相变过程中形成的。     

稀土催化体系催化PET固相缩聚的研究

研究了稀土催化体系对聚对苯二甲酸乙二酯固相缩聚反应的催化效果及对所得高分子量聚酯切片性能的影响,发现稀土催化体系可明显提高聚酯固相缩聚的反应速率,稀土催化体系对聚酯固相缩聚反应的催化活性明显高于传统催化体系,其中单一稀土催化体系与混合稀土催化体系在较低温度下具有相近的催化活性,而在较高温度下单一稀土催化体系的催化活性较高;加入稳定剂,不影响稀土催化的固相缩聚反应速率,稀土催化固相缩聚得到的PET样品具有较高的结晶度和较大的晶粒尺寸,其中单一稀土催化所得样品的晶粒尺寸最大,相应地,单一稀土催化的固相缩聚反应活化能也最大;稀土催化体系催化聚酯固相缩聚反应时添加适当稳定剂,可获得与采用传统催化体系得到的PET切片相近的热稳定性。     

NdFeB合金选择氢爆的研究

对NdFeB合金的选择氢爆进行了研究。研究表明，在较低的环境温度和氢气压力下，通过事先对合金中富Nd相的吸氢量进行理论计算并对放人容器内的NdFeB合金量进行定量控制，NdFeB合金在吸氢过程中完全可以实现良好的选择氢爆。SEM观察表明，选择氢爆时其碎裂的方式均为沿晶断裂，爆裂后粉末中的主相晶粒均是单晶粒子，Nd2Fe14B主相晶粒内均无裂纹形成。与完全氢爆相比，选择氢爆后的晶粒较粗大，且较均匀，但细小晶粒较少。     

聚苯硫醚/尼龙6共混物界面对结晶行为的影响

高分子作为材料时 ,其力学性能受其结晶形态的影响 ,而其结晶形态与其结晶行为有关 .结晶性聚合物共混物中结晶组分由于第二组分存在 ,改变了结晶组分在熔体时的化学与物理环境 .因此 ,其结晶组分的结晶行为不仅取决于两组分在熔体时的相容性 ,而且与第二组分是否起到异相晶核作用和 /或两组分间界面是否诱导成核作用有关 ,从而影响共混物中结晶组分的结晶行为 ,导致共混物力学性能的改变[1～ 4] .在ＰＰＳ/ＰＡ6共混物中 ,由于ＰＰＳ的熔点和熔体结晶温度都比ＰＡ6的高 ,共混物熔体降温结晶ＰＰＳ是在ＰＡ6熔体存在下发生结晶 ,而ＰＡ6是在…     

Delamination of Organically Modified Layered Filler via Solid‐State Processing

Summary: Solid‐state processing for the preparation of poly(p‐phenylenesulfide) (PPS‐) based nano‐composites having finely dispersed layered fillers was conducted. The mixture of PPS and organically modified layered filler (OMLF) (95/5 wt./wt.) was subjected to the processing using thermostated hot‐press at 150 °C, below T_m of PPS (i.e., PPS is still at the solid‐state), and applying pressures of 33 MPa for 30 s. The mixture exhibited disorder and delaminated layer structure with the thickness of 10–20 nm into the PPS matrix. In contrast, a nano‐composite prepared by melt compounding at 300 °C for 3 min showed large stacked silicate layers in the PPS matrix. The processing led to delamination of the silicate layers and attained the discrete dispersion.

TEM bright field image and FFT spectrum of a solid‐state processed PPS nano‐composite.     

STUDIES ON THE EXCIMER FLUORESCENCE AND THE STERIC TACTICITY OF POLYPHENYLSILSESQUIOXANES

The steric tacticity of polyphenylsilsesquioxanes (PPS) was studied by exeimer fluorescence spectroscopy. It was found that the fluorescence of PPS come mainly from its intramolecular excimers, The experimental results indicated that the steric-structure of PPS is most probably cisisotactic rather than the cis-syndiotactic as suggested in the literature. With the increase in defect content monomer fluorescence intensity increases because of the enhanced mobility of phenyl groups. Molecular weights and molecular weight distributions do not affect the fluorescence spectra of PPS.     

CaF2：Ce^3＋中的电荷补偿问题的探讨

在不同的反应条件下,运用固相反应的方法合成了CaF_2∶Ce~(3+)多种粉末磷光体,测定了它们的荧光光谱,发现了3种不同的发光中心,并探讨了3种发光中心的转化规律;研究了不同阳离子电荷补偿剂对CaF_2∶Ce~(3+)光谱性质的影响;指出了不同发光中心的产生是电荷补偿途径不同所致。     

Editorial

The curing and degradation behaviour of poly(phenylene sulphide) (PPS) and poly(2-methyl phenylene sulphide) (PMPS) in air and nitrogen has been studied. Curing studies have been made utilising assessment by solubility, indentation hardness, dynamic mechanical properties and heat of crystallisation studies. The results are critically discussed in terms of their ability to assess the degree of curing achieved.Degradation studies with product analysis by gas-liquid chromatography, infrared spectroscopy and chemical tests are reported and mechanisms of curing and degradation suggested and tested by studies on possible intermediates. The degradation behaviour of PMPS is complicated by oxidative and thermal reactions associated with the methyl substituent.     

Time-resolved EPR and laser photolysis investigations of photoinduced ω-bond dissociation in an aromatic carbonyl compound having triplet π,π* character

Photochemical properties of photoinduced ω-bond dissociation in p-phenylbenzoylbenzyl phenyl sulfide (PPS) having the lowest triplet state (T₁) of π,π* character in solution were investigated by time-resolved EPR and laser flash photolysis techniques. PPS was found to undergo photoinduced ω-bond cleavage in the excited lowest singlet state (S₁(n,π*)) with a quantum yield (Φ_rad) of 0.15 for the radical formation, which was independent of excitation wavelengths. Based on the facts of the observation of the absorption spectrum of triplet PPS upon triplet sensitization of xanthone, and absence of CIDEP signal, ω-cleavage was shown to be absent in the T₁(π,π*) state of PPS. Considering the electronic character of the excited and dissociative states of PPS, a schematic energy diagram for the ω-bond dissociation of PPS was shown.     

Large scale synthesis of red emissive carbon dots powder by solid state reaction for fingerprint identification

Red emissive carbon dots(CDs) powder was synthesized on a large scale from phloroglucinol and boric acid by a novel solid state reaction with yield up to 75%. This method is safe and convenient, for it needs neither high pressure reactors nor complicated post-treatment procedures. The as-prepared carbon dots powder exhibited strong red fluorescence with excitation-independent behavior. XPS measurement and PL spectra suggest that such red fluorescence arise from boron-doped structures in CDs, which increases along with the boron concentration on CDs surface but decreases when the concentration quenching effect takes place. To overcome the aggregation induced fluorescence quenching of the solid CDs powder,the conventional methods are dispersing CDs into a large amount of inert substrates. But our present work provides a new strategy to realize strong red fluorescence of CDs in solid state. As a result, such carbon dots powder works well for latent fingerprint identification on various material surfaces.     

聚苯硫醚及其聚醚砜共混物结晶动力学的研究

本文采用DSC方法,研究了聚苯硫醚及其聚醚砜共混物的等温结晶动力学。结果表明,经α-氯代萘处理后的聚苯硫醚原粉结晶速率常数有明显提高;聚苯硫醚/聚醚砜共混物的Avrami指数较纯聚苯硫醚低,共混物的结晶速率常数随共混组成变化出现最低值;共混物存在明显的二次结晶现象,t_(?)与t_(max)之间存在线性关系。     

动态弹簧分析法的改进及其在研究环氧树脂固化过程中的应用

在文献的基础上改进了动态弹簧分析法,提高了测试精度,使此法不但适用于高聚物的高弹态而且也适用于它的玻璃态。 将改进了的动态弹簧分析法试用于环氧树脂的等温固化过程的研究,测定了等温固化过程中环氧树脂动态贮能模量和内耗的变化曲线,并进行了表观动力学分析。