环氧树脂和石墨对高氯酸钾类烟火药撞击感度的影响

为了揭示高氯酸钾类烟火药的安全性,制备了本工作称为样品1#～7#的7种50/50/m/n-KClO4/Al/环氧树脂/石墨混合物体系(m=n=0;m=3,n=0;m=5,n=0;m=5,n=1;m=5,n=2;m=5,n=3;m=5,n=4)。用GJB772A-1997-601.1,热重-差热分析(TG-DTA)和扫描电子显微镜(SEM)研究了环氧树脂和石墨对高氯酸钾类烟火药撞击感度的影响。结果表明:样品1#～7#的撞击感度爆炸百分数分别为0,60,76,40,12,2和0。与样品1#比较,样品1#中加入环氧树脂使样品2#和3#的撞击感度爆炸百分数升高,且随样品1#中环氧树脂含量的增加,撞击感度爆炸百分数升高。与样品3#比较,样品3#中加入石墨使样品4#～7#的撞击感度爆炸百分数降低,且随样品3#中石墨含量的增加,撞击感度爆炸百分数以4#>5#>6#>7#次序降低。探讨了环氧树脂对KClO4/Al二元体系起增感作用和石墨起减感作用的原因。     

YBa_2Cu_3O_(7-y)超导体合成机理

采用 TG-DTA 热分析和 X 射线衍射相结合的方法,研究了由不同原料制取单一相 YBa2-Cu_3O_(7-(?))超导体的合成反应机理。试验结果表明,YBa2Cu_3O_(7-(?))的形成经历两个反应阶段,首先形成 BaCuO_2和 Y_2Cu_2O_5,随后这两个二元复合氧化物化合形成 YBa2Cu_3O_(7-(?))。各步反应温度受钡盐种类控制,采用 Ba(NO_3)_2原料,在750℃即可表现出超导性,T_c 达86K。     

Synthesis of Titania Pillared Saponite in Aqueous Solution of Acetic Acid

The preparation of TiO₂-pillared saponite was carried out in a CH₃COOH aqueous solution. Titanium ion species to intercalate into the interlayer of saponite were obtained by an addition of Ti(C₃H₇O)₄ to an aqueous solution of CH₃COOH and by subsequent aging of the solution for a prescribed time. Ti⁴⁺-intercalated saponite including organic materials was obtained by ion exchange. After the sample was calcined at 500°C in air, TiO₂-pillared saponite was obtained. The resulting TiO₂-pillared saponite (Ti-Sapo) possessed surface areas in the range 300–400 m²/g and a sharp pore size distribution with the pore radius of 1.2 nm. The basal spacing of the product heated at temperature >250°C was about 2.45 nm. The pillar height of TiO₂ in the Ti-Sapo was estimated to be 1.5 nm.     

染料中性蓝BNL对黑索金热分解的影响

黑索金(环三次甲基三硝胺)的热分解特性与推进剂的燃烧性能密切相关,添加少量催化剂是调节推进剂燃烧性能的有效方法.用TG-DTA法测定了黑索金的热分解性能,利用TG-DTA曲线分析了染料中性蓝BNL对黑索金热分解的影响,并进行了热分解动力学研究,利用Kissenger法计算得到了黑索金在加入染料中性蓝BNL前后的热分解反应活化能.结果表明.染料中性蓝BNL对黑索金的热分解表现出了较好的催化活性,使黑索金的分解过程提前.     

粒径与加热速度对金属Al氮化过程的影响

在氮气流量为55 ml/min条件下,分别以5,10,15 ℃/min的加热速率对不同粒径(d_(50)为62,29,7.5μm)的金属Al粉进行了TG-DTA分析和反应活化能的研究.结果表明:在相同的实验条件下,随Al粉粒径的减小和加热速率的增大,生成AlN的反应活化能降低;在N_2流量55 ml/min和加热速率5 ℃/min条件下,d_(50)= 29 μm和d_(50) =7.5 μm Al粉生成AlN的主放热峰温比d_(50) =62 μm Al粉的分别可降低140和250 ℃.在N_2流量55 ml/min条件下,d_(50)= 7.5 μm Al粉以10和15 ℃/min为加热条件的氮化反应速率比5 ℃/min的提高0.9和1.7倍.Al粉反应生成AlN的全过程,主要由界面反应和内扩散反应交替完成,且整个反应过程应为扩散机制控制.     

有机大阳离子与HnXW12O40·nH2O（X=B，Si，P）多金属氧酸盐的合成及热行为

合成了3种新的多金属氧酸盐(CTMA)5BW12O40·8H2O,(CTMA)4SiW12O40·3H2O,(CTMA)3PW12O40·2H2O,利用元素分析、IR光谱和TG-DTA技术对其进行了表征.IR光谱表明这些化合物不仅含有Keggin型结构,而且存在有机大阳离子的特征吸收峰;TG-DTA曲线显示它们的热行为是一个多步分解过程,首先这些化合物在大约269℃以下脱去水分子,然后它们的无水多金属氧酸盐经历了两步或3步的分解过程,分别脱去CTMA分子及其碎片,并伴随Keggin型结构的塌陷.通过XRD和IR光谱确证其最终分解产物是一个含有WO3与B2O3,SiO2或P2O5的混合物.同时还提出了这些化合物可能的热分解过程.     

A simple strategy to synthesize and characterization of zirconium modified PCs/γ–Al_2O_3

Crystalline phase is the key factor for catalyst activity. The zirconium modified PCs/γ-Al_2O_3 samples were prepared through a simple step incipient-wetness impregnation method. The raw materials and samples were characterized by thermogravimetric-differential analysis(TG-DTA), X-ray diffraction(XRD), Fourier transform infrared spectroscopy(FT-IR), temperature-programmed desorption of ammonia and carbon dioxide(NH_3-and CO_2-TPD). The effects of calcination temperature and zirconium content on structure, chemical transformation,and acidity-basicity were investigated. Calcination temperature exhibited the major effect on the crystalline phase of samples. The new phase of Al0.1Zr_(0.9)O_(1.95) was exhibited which was above 650 ℃. In addition, zirconium content was influenced by the acidic and basic properties of the surface. The acidity and basicity of the Zr PCs/γ-Al_2O_3 sample increased with the increasing of zirconium content.     

Investigations of surface characterization of silicone rubber due to tracking phenomena under a.c. and d.c. voltages

In the present work, tracking phenomena has been studied with silicone rubber material under the a.c. and d.c. voltages following IEC-587 standards. The surface condition of the tracked zone was analysed using wide angle X-ray diffraction (WAXD) and thermogravimetric differential thermal analysis (TG-DTA) studies. The tracking time was different for a.c. and d.c. voltages.     

氮化镍钨加氢精制催化剂氮化过程的TG—DTA研究

通过对镍钨单金属氧化物、双金属氧化物、负载型金属氧化物和工业镍钨系列G1催化剂在氢氮混合气中还原氮化和钝化过程的TG-DTA原位实验,分别考察了反应温度、氢氮比、中间产物、助剂等因素对镍钨金属氧化物氮化历程的影响。结果表明,WO3可以在氢氮混合气中被还原氮化;氮化反应分两段进行;在氢氮体积比(4～5)∶1,反应温度650℃的条件下,WO3可以被还原为产物W2N;在不同氢氮比的混合气中氮化,WO3会生成不同的中间产物WO2和WOXNY,中间产物WOXNY进一步氮化生成W2N要比WO2容易;助剂Ni的加入使氮化反应温度降低了100℃;载体γ-Al2O3的加入使金属氧化物的氮化过程变为一步氮化还原反应。氮化产物W2N在通常条件下只会与空气中的氧发生表层氧化,而不会发生剧烈的氧化燃烧。因此,对于氮化产物W2N不必进行钝化处理。利用氮化处理技术,可以对现有工业催化剂进行氮化处理。     

用超临界二氧化碳法合成偶氮苯-环糊精纳米复合体

以超临界二氧化碳为溶媒，将偶氧苯分子插入到α-以及β-环糊精的分子环空洞中合成出了偶氧苯-环糊精纳米复合体。环糊精与偶氧苯的摩尔分子为1：1的混合物，放入压力30MPa、温度120℃的超临界装置中处理后，对其生成物采用红外、固体核磁共振、X-射线衍射、差热分析及化学元素分析等手段进行了分析，结果表明偶氧苯成功地插入到β-环糊精分子环空洞中形成了纳米复合体，而α-环式糊精与偶氮苯之间只是简单的物理混合物，没有形成纳米复合体。所得到的偶氮苯-β-环式糊精复合体具有通道式分子结构：二个β-环式糊精分子捕获一个偶氧苯分子，β-环式糊精的分子环空洞连成一个通道。偶氧苯插入到β-环式糊粉分子环空洞中后其热稳定性也得到大幅度提高。