水热法制备负热膨胀性ZrW2O8粉体

用水热法并经570 ℃热处理6 h制备了ZrW2O8粉体,对水热法制备的前驱体进行了热重-差热分析.用X射线粉末衍射、扫描电子显微镜对ZrW2O8粉体的微观结构及形貌进行表征,结果表明:ZrW2O8粉体为单一α-ZrW2O8相,粉体颗粒为规则的长方体棒状,尺寸约为1.2μm×1.2μm×10μm.原位X射线粉末衍射分析表明:所得ZrW2O8粉体具有很好的负热膨胀特性,从室温到500 ℃,其热膨胀系数为-6.30×10-6 ℃-1;在150～175 ℃温度范围内发生了α-ZrW2O8向β-ZrW2O8相的转变.     

S油田W南区长6特低渗透储层物性下限标准研究

鄂尔多斯盆地S油田W南区长6储层孔隙度的集中分布范围在10%~12%,渗透率集中分布范围在(0.1~0.5)×10-3μm2,属典型的低孔、特低渗储层。结合静态、动态资料及岩石物理实验,综合利用物性试油法、试油资料约束法、油水相对渗透率法、压汞分析法、压汞参数法等5种方法,确定了该储层有效物性下限孔隙度为10%、渗透率为0.15×10-3μm2,为有效储层划分及储量计算提供了依据。     

A self assembled monolayer based microfluidic sensor for urea detection

Urease (Urs) and glutamate dehydrogenase (GLDH) have been covalently co-immobilized onto a self-assembled monolayer (SAM) comprising of 10-carboxy-1-decanthiol (CDT) via EDC-NHS chemistry deposited onto one of the two patterned gold (Au) electrodes for estimation of urea using poly(dimethylsiloxane) based microfluidic channels (2 cm × 200 μm × 200 μm). The CDT/Au and Urs-GLDH/CDT/Au electrodes have been characterized using Fourier transform infrared (FTIR) spectroscopy, contact angle (CA), atomic force microscopy (AFM) and electrochemical cyclic voltammetry (CV) techniques. The electrochemical response measurement of a Urs-GLDH/CDT/Au bioelectrode obtained as a function of urea concentration using CV yield linearity as 10 to 100 mg dl(-1), detection limit as 9 mg dl(-1) and high sensitivity as 7.5 μA mM(-1) cm(-2).     

Tm3+掺杂硅酸盐玻璃的1.8μm光谱性质

研究了Tm掺杂硅酸盐玻璃的热稳定性、1.8μm荧光性质.测试了玻璃样品的特征温度、吸收光谱和荧光光谱:根据吸收光谱,计算并讨论了玻璃样品的吸收和发射截面、Judd-Ofelt参数、辐射跃迁几率和辐射寿命等光谱参量.计算得出Tm3+:3F4→3H6能级跃迁的辐射寿命达到5.62ms,受激发射截面和辐射寿命的乘积σem×τ...     

Thin layer drying kinetics of by-products from olive oil processing

The thin-layer behavior of by-products from olive oil production was determined in a solar dryer in passive and active operation modes for a temperature range of 20-50 °C. The increase in the air temperature reduced the drying time of olive pomace, sludge and olive mill wastewater. Moisture ratio was analyzed to obtain effective diffusivity values, varying in the oil mill by-products from 9.136 × 10(-11) to 1.406 × 10(-9) m(2)/s in forced convection (m(a) = 0.22 kg/s), and from 9.296 × 10(-11) to 6.277 × 10(-10) m(2)/s in natural convection (m(a) = 0.042 kg/s). Diffusivity values at each temperature were obtained using the Fick's diffusion model and, regardless of the convection, they increased with the air temperature. The temperature dependence on the effective diffusivity was determined by an Arrhenius type relationship. The activation energies were found to be 38.64 kJ/mol, 30.44 kJ/mol and 47.64 kJ/mol for the olive pomace, the sludge and the olive mill wastewater in active mode, respectively, and 91.35 kJ/mol, 14.04 kJ/mol and 77.15 kJ/mol in natural mode, in that order.     

高效液相色谱测定40%乙烯利中6-苄氨基嘌呤方法的研究

首次建立了高效液相色谱测定40%乙烯利中6-苄氨基嘌呤含量的方法.色谱柱为Symmetry C18(150 mm×3.9 mm×5 μm);流动相为甲醇-水(V/V=50:50);流速为0.8 mL/min;线性回归方程为y=9.35×106x-3.52×103,r=0.999 8,线性范围为32.9～411 μg;加标回收率平均值为98.2%,RSD为1.42%.     

疏水改性氧化石墨烯/环氧复合涂料的制备及其防腐性能研究

以叔碳酸缩水甘油酯(E-10P)为疏水单体,通过环氧与羧酸的共价键合,在氧化石墨烯(GO)表面引入疏水性支化碳链,改性后的氧化石墨烯(F-GO)作为防锈填料加入环氧树脂中得到F-GO/环氧复合涂料。通过红外光谱、拉曼光谱、X-射线衍射、热重分析对F-GO的结构进行表征,通过场发射扫描电镜观察F-GO及复合涂料的微观形貌,并通过电化学阻抗、极化曲线和盐雾试验测试了复合涂料的防腐性能。结果表明:E-10P可利用其空间效应阻碍片层的团聚;疏水效应可提高F-GO的热稳定性和与环氧树脂的相容性;与空白环氧涂层相比,当复合涂料中F-GO质量分数为0.2%时,厚度为20~25 μm的防腐涂层的腐蚀电流可由2.358 6×10 ^-6 A/cm ²下降至2.000 2×10 ^-11 A/cm ²,阻抗值可由1.1×10 ⁷ Ω·cm ² 提升至6.9×10 ⁹ Ω·cm ²。     

Controlled synthesis of ultra-long AlN nanowires in different densities and in situ investigation of the physical properties of an individual AlN nanowire

The controlled synthesis of different growth densities of ultra-long AlN nanowires has been successfully realized by nitridation of Al powders for the first time. These AlN nanowires have an average diameter of about 100 nm and their mean length is over 50 μm. All the synthesized ultra-long nanowires are pure single crystalline h-AlN structures with a growth orientation of [0001]. We preferred the self-catalyzing vapor-liquid-solid (VLS) mechanism to illustrate their growth process. Although the sample with the middle growth density (3.2×10(7) per cm2) of AlN nanowire performs the best field emission (FE) properties, the emission uniformity is not good enough for field emission display applications, which may be attributed to their low intrinsic conductivity. Moreover, the electrical transport and FE properties of an individual ultra-long AlN nanowire are further investigated in situ to find the decisive factor responsible for their FE behaviors. An individual AlN nanowire is observed to have a mean 1 nA field of 440 V μm(-1) and 1 μA field of 480 V μm(-1) as well as an average electrical conductivity of about 2.7×10(-4)Ω(-1) cm(-1), which is lower than that of some cathode materials with excellent FE properties. Therefore we come to the conclusion that the electrical conductivity of the AlN nanowire must be improved to a higher level by some effective ways in order to realize their practical FE device applications.     

CO_2微孔发泡聚碳酸酯/聚苯乙烯

采用快速升温法,在相对较低的压力下制备聚碳酸酯(PC)/聚苯乙烯(PS)共混物的微孔发泡材料.获得的PC/PS共混物发泡材料的平均泡孔直径为4.3μm,泡孔密度为8.89 × 10~9个/cm~3,而在相同条件下制得的PC和PS发泡材料的平均泡孔直径分别为28.6μm和143.8 0μm,泡孔密度分别为2.23×10~7个/cm~3和3.6×10~5个/cm~3.并研究PC、PS和PC/PS共混物的CO_2吸附行为以及PC/PS共混物在不同温度下的泡孔形态,发现泡孔首先在PS相中成核并生长.     

高效液相色谱法测定6-APA的相关物质

采用高效液相色谱法测定6-APA中可能存在的杂质。方法按照《中国药典》2010年版。流动相为0.1 mol/L磷酸盐缓冲液乙腈（80∶20）,稀释液为pH=5.5的磷酸盐缓冲液,流速为1.0 mL/min,检测波长为224 nm,进样量为20μL,柱温为35℃。结果表明,该检测方法具有较强专属性,线性很好,杂质A、B的相关系数分别为0.999 4、0.999 1,准确回收率分别为98.1%、95.8%,定量限分别为9.992 6×10-8、1.004 8×10-7,检测限分别为3.330 9×10-8、3.349 1×10-8,杂质的相关条件符合规定。该方法简便、易行,结果准确。     

Growth and Spectral Properties of Sm^（3＋）：YAl3（BO3）4 Crystal

采用助熔剂法生长高质量的Sm3＋：YAl3（BO3）4晶体,并通过吸收光谱、荧光光谱对它的光谱特性进行表征,采用Judd–Offelt理论分析了该晶体的光谱参数。结果表明：Sm：YAl3（BO3）4晶体的t（t=2,4,6）参数分别为2=0.058×10–20,4=1.28×10–20,6=1.06×10–20。6H7/2能级的辐射寿命为520.2μs。热学性能测试表明：Sm：YAl3（BO3）4晶体具有较高的热导率,沿c轴方向是5.30W/（m K）。     

Continuous electrodeposition for lightweight, highly conducting and strong carbon nanotube-copper composite fibers

Carbon nanotube (CNT) fiber is a promising candidate for lightweight cables. The introduction of metal particles on a CNT fiber can effectively improve its electrical conductivity. However, the decrease in strength is observed in CNT-metal composite fibers. Here we demonstrate a continuous process, which combines fiber spinning, CNT anodization and metal deposition, to fabricate lightweight and high-strength CNT-Cu fibers with metal-like conductivities. The composite fiber with anodized CNTs exhibits a conductivity of 4.08 × 10(4)-1.84 × 10(5) S cm(-1) and a mass density of 1.87-3.08 g cm(-3), as the Cu thickness is changed from 1 to 3 μm. It can be 600-811 MPa in strength, as strong as the un-anodized pure CNT fiber (656 MPa). We also find that during the tensile tests there are slips between the inner CNTs and the outer Cu layer, leading to the drops in electrical conductivity. Therefore, there is an effective fiber strength before which the Cu layer is robust. Due to the improved interfacial bonding between the Cu layer and the anodized CNT surfaces, such effective strength is still high, up to 490-570 MPa.     

铈模拟放射性废物固化体的物理化学性质

以稀土元素Ce作为示踪核素,采用铝热剂自蔓延高温合成技术固化了粒度≤200μm的模拟核废物土壤,通过密度测定和扫描电子显微镜、X射线荧光光谱、X射线衍射、电感耦合等离子发射光谱分析,研究了不同Ce含量的固化体的组成结构和核素浸出率。结果表明：在CeO2质量分数大于1%的情况下,示踪核素Ce主要是以CeAl11O18和Ce2SiO5的矿物晶体的形态存在于固化产物中。产物为无定形态玻璃和陶瓷体的混合物,体积密度超过3.0 g/cm3。固化体中示踪核素Ce的28 d平均浸出速率为10-5～10-6 g/（m2.d）,比一般硼硅酸盐玻璃固化体中稀土元素的浸出速率低1～2个数量级。固化体中Ca、Si和Al的28d浸出速率约为10-3g/（m2.d）,Fe的28d浸出率约为10-4g/（m2.d）。     

三元层状氮化物Ti_4AlN_3材料的合成及微观结构研究

以Ti、Al、TiN粉为原料,采用热压烧结工艺在1400 ℃合成了含少量TiN和Al_3Ti的Ti_4AlN_3块体材料,分别研究了不同原料配比、烧结温度及合成时间下烧结试样的相组成.混合粉Ti/1.2Al/3TiN在1400 ℃下保温2 h所得烧结试样经背散射电子像结合EDS能谱分析,证实成功合成了Ti_4AlN_3材料.烧结试样晶粒尺寸为5～10 μm,晶体呈层状或板状结构,结晶良好,结构致密.相对密度达到99.3%,维氏硬度及电导率分别为3.9～5.1 GPa和1.2×10~6 Ω~(-1)·m~(-1),表明其具有优良的机械加工及导电性能.     

Length dependent foam-like mechanical response of axially indented vertically oriented carbon nanotube arrays

The axial compressive mechanical response of substrate-supported carbon nanotube (CNT) arrays with heights from 35 to 1200 μm is evaluated using flat punch nanoindentation with indentation depths to 200 μm. The compressive behavior is consistent with that of an open-cell foam material with array height playing a role similar to that of occupation density for traditional foam. Mechanical yielding of all arrays is initiated between 0.03 and 0.12 strain and arises from localized coordinated plastic buckling. For intermediate CNT array heights between 190 and 650 μm, buckle formation is highly periodic, with characteristic wavelengths between 3 and 6 μm. Buckle formation produced substantial force oscillations in both the compressive and lateral directions. The compressive elastic modulus of the arrays is obtained as a continuous function of penetration depth and attains a value between 10 and 20 MPa for all arrays during mechanical yield. A qualitative model based upon concepts of cellular foam geometry is advanced to explain the observed CNT buckling behavior.     

多步组装合成介孔二氧化硅担载膜

采用浸渍法和表面改性多步组装合成技术在商业用多孔氧化铝管上制备介孔二氧化硅担载膜。所制备的介孔二氧化硅膜层的厚度平均为2μm,平均孔径为1.59nm。单一气体的渗透实验表明:气体通过介孔二氧化硅膜层符合Knudsen扩散模型,在298K和100kPa的恒定条件下,氦气和氮气的渗透量分别为15.6×10-6mol/(s·m2·Pa)和2.5×10-6mol/(s·m2·Pa)。渗透蒸发实验表明:经六甲基二硅氮烷表面改性的二氧化硅膜层在303K和313K下分别对含3%(质量分数,下同)和5%乙醇的水溶液进行乙醇组分的提浓,乙醇的分离系数和渗透通量分别为15.2～18.7和1.09～1.25kg/(m2·h)。     

低温油藏深部调驱用弱凝胶体系研究

针对低温油藏深部调驱需要,在1%的醋酸铬溶液中,加入杀菌剂DQ、助剂DW,得低温交联剂,与聚合物混合均匀,30℃下反应,得有机弱凝胶。结果表明,在聚合物KYPAM2浓度为2 000～3 000 mg/L,聚合物/交联剂质量比为8∶1～10∶1,体系矿化度5 000～10 000 mg/L,30℃的油藏温度条件下,30 d后弱凝胶强度可达到10 000 mPa.s以上,未出现脱水、破胶的现象,并表现出良好的长期稳定性;在3 500×10-3μm2和560×10-3μm2填砂管组成的并联模型上,弱凝胶体系优先进入高渗通道,使后续流体转向进入低渗岩心,改善了非均质油藏开发效果。     

氢氧化镁纳米棒的等温分解动力学研究

以六水氯化镁和轻质氧化镁为原料,制备出碱式氯化镁纳米棒;再以碱式氯化镁纳米棒为前驱物,采用沉淀转化法,合成出直径约100—200nm,长约6～10μm的氢氧化镁纳米棒。利用热分析法对氢氧化镁纳米棒进行了等温热分解动力学研究,结果表明,氢氧化镁纳米棒在300℃和350℃时的热分解反应服从随机成核和随后生长机理、积分机理函数g（α）=[-ln（1-α）]^1/m,表观活化能E=153kJ／mol,指前因子A=5．83×10^12s^-1。     

高效液相色谱-串联质谱法测定油辣椒中罗丹明B

建立了油辣椒中罗丹明B的高效液相色谱-串联四极杆质谱联用测定方法,该方法经乙腈提取样品,以waters-C18柱（2.1×50mm,1.7μm）分离,流动相为甲醇-0.1%甲酸水,电喷雾正离子MRM模式检测。方法检出限0.1ng/mL,线性范围0.1μg/L～10μg/L,加标回收率99.5%～106.4%,相对标准偏差为1.08～3.07%。     

高效液相色谱法测定工业废水中盐酸苯肼

通过实验建立了工业废水中盐酸苯肼的高效液相色谱分析方法。色谱条件为:Kromasil-C18(150 mm×4.6 mm,5μm)色谱柱,流速1 mL/min,柱温30℃,进样体积10μL,流动相为V(甲醇)∶V(8 mmol/L KH2PO4+4 mmol/LK2HPO4)=35∶65,测定波长235 nm。测定结果表明,线性范围为0.1～100 mg/L,平均加标回收率为98.2%,相对标准偏差为1.06%。该方法操作简单,分析快速、准确。