膨胀石墨的尺寸效应及对细鳞片石墨的影响

为提高细鳞片膨胀石墨的理化性能,作者用不同粒度的鳞片石墨在相同酸氧化条件下制备可膨胀石墨,经膨胀后发现:随粒度减小,石墨膨胀容积均在逐渐减小.通过电镜扫描和元素微区分析形貌结构和成分,发现随粒度减小,插入量变小,其结构也呈相应变化;证实可膨胀石墨与膨胀石墨均存在尺寸效应.它对细鳞片石墨膨胀性能、高温热失重性能及导热性能等有较大影响.     

再次插入法制备超大膨胀体积石墨层间化合物(英文)

为进一步增大膨胀石墨的膨胀体积,用二次插入的方法制备了石墨层间化合物。首先用化学氧化法制备了膨胀体积为250mL/g的可膨胀石墨,然后以膨胀体积为250mL/g的可膨胀石墨为原料,用二次插入的方法制备了膨胀体积为380mL/g的膨胀石墨。讨论了各种反应物比率、反应温度和反应时间对膨胀体积的影响。对制得的膨胀石墨进行了各种表征,XRD谱显示产物保持了天然石墨的层状晶体结构,但是产物的石墨层间距离增大。扫描电镜照片显示通过二次插入石墨层间确实被进一步打开。结果显示这种新的制备方法是可行的,它为纳米石墨材料的研究提供了新的思路。     

原料粒度对石油焦基活性炭性能的影响

以不同粒度范围的石油焦为原料,KOH为活化剂,采用化学活化工艺制备了超级电容器用活性炭电极材料.采用N2吸附法表征了活性炭材料的BET比表面积及孔结构;在1mol/L的Et4NBF4/AN有机电解液体系下组装成模拟电容器,并考察了活性炭材料的电化学性能.结果表明:随着原料粒度的减小,活性炭的振实密度和收率先增大,然后再减小.原料粒度范围越窄,活性炭具有越小的BET比表面积和孔容.在1mol/L的Et4NBF4/AN电解液体系下,随着石油焦粒度的不断减小,活性炭材料的质量比容量不断增大,在粒度<38μm时取得最大值140F/g.粒度为38～44μm的石油焦制备出的活性炭在1A/g电流下质量比容量为126.6F/g,在20A/g电流下质量比容量为116.2F/g,容量衰减只有8.2%,表现出良好的功率特性.     

石蜡/不同粒径膨胀石墨复合相变储热材料的制备和性能

用熔融共混法制备石蜡/不同粒径膨胀石墨复合相变储热材料,对样品进行XRD、FT-IR、SEM、DSC和LFA表征分析,研究了不同粒径膨胀石墨的质量比例对复合相变储热材料性能的影响。结果表明:随着小粒径膨胀石墨含量的增加,复合相变储热材料的热扩散系数先增大后减小。在大小粒径膨胀石墨质量比例为9∶1时,石蜡充分利用了大小粒径膨胀石墨的镶嵌式空间结构,复合相变材料的热扩散系数为1.964×10-6m2/s,比纯石蜡提高了22倍,相变潜热为144.2 J/g。     

不同粒径膨胀石墨的制备及其微观结构

对化学法制备膨胀石墨的工艺条件的选择进行了分析,以硝酸与磷酸的混酸为插层剂、高锰酸钾为氧化剂制备出了不同粒径的膨胀石墨,利用正交实验和平行实验确定了最佳工艺条件;研究了石墨粒度效应对氧化剂用量的影响;并对不同粒径膨胀石墨的微观结构进行了研究。研究结果表明,制备大鳞片膨胀石墨的最佳工艺为：石墨与混酸的质量体积比为1：4,...     

化学氧化法制备可膨胀石墨过程中的电位控制

以高锰酸钾、硫酸、天然鳞片石墨为原料,采用化学氧化法制备可膨胀石墨。通过调控体系初始氧化还原电位,并结合其膨胀容积值,探讨石墨氧化的最佳电位区间,采用扫描电镜及X射线衍射仪对样品进行表征。结果表明,当体系初始氧化还原电位为1340~1810mV时,能够获得平均膨胀容积大于230mL/g,最高300mL/g的可膨胀石墨,扫描电镜及X射线衍射结果证实了此区间的合理性。此法避免了传统化学氧化法通过复杂正交实验来确定最佳工艺的弊端,可为实现可膨胀石墨制备的自动化和工业化生产提供重要的理论依据。     

低温加热快速制备膨胀石墨（英文）

本文提出了一种简单、节能、高效的膨胀石墨制备方法。以鳞片石墨为原料,K_2S_2O_8为膨胀剂,在80℃的条件下,加热数分钟即可快速制备出膨胀石墨。采用XRD、SEM、FTIR、Raman和四探针对样品的结构、形貌、官能团和导电性能进行了表征。结果表明,石墨由鳞片状转变为蠕虫状,最大膨胀容积为150 mL/g,且该方法对石墨结构的氧化程度低。由该膨胀石墨制备的柔性石墨的电导率为5.47×10~4S/m。该方法因其简单、成本低、对环境危害小等特点具有良好的应用前景。     

细鳞片石墨层间化合物插入量的研究

用不同粒度（60～180目）的石墨在相同条件下制备可膨胀石墨和同一粒度的石墨在不同酸化条件下制备可膨胀石墨，通过差量法和元素分析对石墨酸化前后总质量及主要元素的量的变化，对粒度和不同酸化条件对可膨胀石墨层间化合物插入量的影响进行了分析。结果表明：插入量随酸化、氧化条件的增强而增加、随粒度的变化不明显。     

低碳细鳞片石墨制备可膨胀石墨的研究

用酸浸泡提纯+H2SO4/H2O2/K2Cr2O7氧化插层体系分步氧化插层复合工艺,以88.22%碳含量、150目的低纯细鳞片石墨制备出可膨胀石墨。研究了浸泡酸、插层剂及分步氧化插层对膨胀体积EV的影响,结合膨胀石墨微观形貌对影响因素进行分析讨论。实验结果表明:用HF预处理2h,H2O2一次氧化1h的鳞片石墨以m(C)∶V(H2SO4)∶m(K2Cr2O7)=1∶4.0∶0.16在超声振荡条件下反应1h,可制备出膨胀体积EV为165mL/g的可膨胀石墨。     

低碳细鳞片石墨制备可膨胀石墨的研究

用酸浸泡提纯+H2SO4/H2O2/K2Cr2O7氧化插层体系分步氧化插层复合工艺,以88.22%碳含量、150目的低纯细鳞片石墨制备出可膨胀石墨。研究了浸泡酸、插层剂及分步氧化插层对膨胀体积EV的影响,结合膨胀石墨微观形貌对影响因素进行分析讨论。实验结果表明:用HF预处理2h,H2O2一次氧化1h的鳞片石墨以m(C)∶V(H2SO4)∶m(K2Cr2O7)=1∶4.0∶0.16在超声振荡条件下反应1h,可制备出膨胀体积EV为165mL/g的可膨胀石墨。     

Electrical and mechanical properties of expanded graphite/high density polyethylene nanocomposites

High density polyethylene (HDPE) were filled with expanded graphite particles that have different particle sizes, 5–7 μm (EG5) and 40–55 μm (EG50) in diameter. Nanocomposites were prepared by the melt-mixing technique using EG5 and EG50 at different weight ratios. Transmission Electron Microscopy (TEM) was used to observe the morphology of the nanocomposites. X-ray diffraction patterns of EG5-HDPE and EG50-HDPE nanocomposites were investigated. Tensile tests were carried out to determine tensile strength, Young’s modulus and elongation at break values. The storage modulus and loss modulus were evaluated by Dynamic Mechanical Analysis (DMA). The effect of EG5 and EG50 on electrical conductivity of HDPE was also determined. The tensile strength of HDPE increased 18.7% and 8.5% when 40 wt% EG5 and EG50 was added into HDPE, respectively. The storage modulus of EG5-HDPE and EG50-HDPE is higher compared to that of HDPE. Incorporation of EG5 and EG10 into HDPE also increased the relaxation transition peak of HDPE. The values of electrical conductivity for EG50-HDPE nanocomposites under the same filler content obtained higher in comparison with those for EG5-HDPE nanocomposites.     

正癸酸-月桂酸-硬脂酸三元低共熔体系/膨胀石墨复合相变材料的制备与表征

将正癸酸(DA)、月桂酸(LA)和硬脂酸(SA)熔融共混制备了三元体系相变材料(DA-LA-SA),以DA-LA-SA为相变材料,膨胀石墨(EG)为载体材料,用熔融共混法制备不同DA-LA-SA含量的三元低共熔脂肪酸/膨胀石墨复合相变材料(DA-LASA/EG-PCMs)。采用FT-IR、XRD、SEM、TGA和DSC对其组成成分、晶体结构、微观形貌、相变温度和相变焓进行表征。结果表明,当DA、LA和SA的质量配比为1∶8∶1时,DA-LA-SA具有较低的相变温度和较高的相变焓;EG由大量的微孔构成,通过微孔束缚和表面吸附与DA-LA-SA物理结合,具有良好的稳定性;EG质量分数为10%时,所制备的DA-LA-SA/EG-PCMs三元相变体系复合相变材料的相变温度为38.6℃,相变焓为123J/g,导热系数为3.572 1 W·(m·K)-1,分散均匀,颗粒粒径较小,具有优良的热性能和稳定性。     

原位反应结合碳化硅多孔陶瓷的制备与性能

以碳化硅(SiC)和氧化铝(Al₂O₃)为起始原料、石墨为造孔剂, 通过原位反应结合工艺制备SiC多孔陶瓷. XRD分析表明多孔陶瓷的主相是SiC, 结合相是莫来石与方石英; SEM观察到多孔陶瓷具有相互连通的开孔结构. 坯体在烧结前后具有很小的尺寸变化, 线收缩率约在±1.5%内. 多孔陶瓷的开口孔隙率随烧结温度和成型压力的增大而减小, 随石墨加入量的增加而增大; 而体密度具有相反的变化趋势. 随着石墨粒径的增大, 多孔陶瓷的孔径分布呈现双峰分布. 抗弯强度随烧结温度和成型压力的增大而增大, 随石墨加入量的增大而减小. 于1450℃保温4h烧成的样品在0～800℃的平均热膨胀系数为6.4×10^-6/K. 多孔陶瓷还表现出良好的透气性、抗高温氧化和耐酸腐蚀性, 但耐碱腐蚀性相对较差.     

Synthesis of high tap density spherical micro-size silver particles by liquid-phase reduction using response surface methodology

Mono-disperse and spherical micro-size silver particles with high tap density were prepared by using silver nitrate as metal source, ascorbic acid as reductant, sulfuric acid as dispersant and polyethylene glycol 4000 (PEG4000) as surfactant. The aim of this paper was to study the simultaneous effects of surfactant dosage (PEG4000/AgNO₃ mass ratio), silver nitrate concentration [AgNO₃], deionized water dosage in reductant solution, stirring rate and their interactions on properties of silver particles. For optimizing these parameters, irregular fractional factorial design of experiments was used. As-prepared silver particles were characterized by X-ray diffraction, scanning electron microscopy, laser particle size analyzer and tap density (tap density refers to the stacking density of particles after vibration compaction) meter. The results showed that silver particles were spherical, mono-disperse and with high tap density (>5.0 g/mL), average particle size of about 2–3 μm and narrow particle size distribution. By surveying the experiment results and analysis of variance, two mathematical models were obtained and optimized parameters were determined. Analysis of the variance demonstrated that the interaction of [AgNO₃] and stirring rate were the most significant factor affecting particle size and PEG4000/AgNO₃ mass ratio and [AgNO₃] were main significant factors affecting tap density. The predicted particle size and tap density were respectively 2.5 μm and 5.065 g/mL while the experimental results were 2.52 μm and 5.108 g/mL, which indicated that the models were in good agreement with the experimental data.     

Characteristics of an artificial graphite anode material for rapid charging: manufactured with different coke particle sizes

An artificial graphite anode material (10–15 μm) is produced using coke at two sizes (10–15 μm, 2–5 μm) and the electrochemical properties are compared and discussed. We produce and measure an artificial graphite anode material using coke with a particle size of 10–15 μm, limited lithium ion insertion–desorption pathways, increased migration pathways, and low-speed charge–discharge characteristics. When a block is manufactured using coke at a particle size of 2–5 μm and an anode material is created with a particle size of 10–15 μm, voids capable of storing lithium ions between the coke particles form inside the anode material. These spaces are utilized and the capacity was measured. In addition, the lithium ion insertion-deintercalation path and lithium ion diffusion distance are controlled and the high-speed discharge properties were measured (78.3%) at low temperatures (5C/0.1C, ? 10 °C). At the same time, the high specific surface area due to the small size of the coke was controlled by the binder pitch used in the block, leading to excellent initial efficiency performance.

     

Percolation Segregation in Binary Size Mixtures of Spherical and Angular-Shaped Particles of Different Densities

Percolation segregation in binary size mixtures for two particulate types, urea (spherical) and potash (angular), were studied. Materials chosen are major raw ingredients of blended fertilizer that represent two extremes based on shape and density. In this study, the coarse and fine particles were classified using particle sizes larger and smaller than 2,000 μm, respectively. Three coarse mean sizes (3,675 μm, 3,075 μm, and 2,580 μm) for both spherical and angular particles and three fines mean sizes (2,180 μm, 1,850 μm, and 1,550 μm) for angular particles and two fines mean sizes (2,180 μm and 1,850 μm) for spherical particles were selected for tests. Size ratio for binary size mixture is defined as the ratio of mean size of coarse to fine particles. Binary mixed samples of coarse and fine particles were placed into the shear box of the primary segregation shear cell (PSSC-II) very gently to avoid segregation. Percolation segregation was quantified using PSSC-II. Based on experimental results, the segregated fines mass, normalized segregation rate (NSR), and segregation rate of fines for binary mixtures were higher for larger size ratios as expected (2.4 > 2.0 > 1.7). The NSR is defined as the amount of fines percolated from initial fines present in the binary mixture based on total time of PSSC-II operation (kg/kg-h). Segregation rate was the highest and lowest for mixing ratios 33:67 and 67:33, respectively, when coarse mean size was 3,675 μm, where mixing ratio for binary mixtures is the ratio of the mass of coarse particles to the mass of fine particles. For the same size ratio, segregated fines mass for coarse-fine size combinations in the binary mixtures of urea and potash were significantly different (p < 0.05). Segregated fines mass of potash and urea particles was significantly different for the same size ratio and the same coarse sizes (p < 0.05). Percent segregated fines of angular particles (59%) was higher than that of spherical particles (45%) for the size ratio 2.0 and coarse mean size of 3,675 μm.     

温度对铁基预合金粉腐蚀泡沫化人造金刚石微粉的影响

采用铁基预合金粉对粒径为40~50μm的人造金刚石微粉进行腐蚀泡沫化处理。研究了不同温度对金刚石微粉表面形貌、颗粒直径、比表面积和孔容积的影响,并对腐蚀图案的各向异性和泡沫化机理进行分析。结果表明:当金刚石和预合金粉质量比为1∶2时,800℃处理的金刚石表面出现明显的腐蚀坑。随着处理温度升高,金刚石泡沫化程度先增大后减小,当处理温度为1 000℃时,金刚石泡沫化效果最好;此时,金刚石的比表面积和孔容积最大,分别为7.322m2/g和0.012mL/g。在腐蚀泡沫化过程中,金刚石发生了石墨化。     

7-氨基-4,6-二硝基苯并氧化呋咱的精制及性能研究

实验室直接制备的7-氨基-4,6-二硝基苯并氧化呋咱的含酸量较高,而炸药的酸度较高非常不利于使用及储存,所以需要对其进行进一步的精制除酸才能安全使用。该文研究采用甲醇、N,N-二甲基甲酰胺(DMF)、二甲亚砜(DMSO)3种溶剂对粗品进行精制,并研究了精制后的样品在含酸量、粒度、微观形貌、机械感度及热安定性方面的性能改变。试验表明,采用甲醇除酸效果最好:精制后的样品pH值为6.6;样品颗粒的尺寸最小,粒度主要分布在0.4~30.0μm,但存在少量的团聚现象;撞击感度和摩擦感度分别为28%和20%;真空安定性测试表明100℃时,真空放气量为0.047 mL/g,200℃时为0.85 mL/g;24 h的热质量损失率为0.80%。