Carbonization behavior of oxidized viscose rayon fibers in the presence of boric acid–phosphoric acid impregnation

The oxidation and carbonization stages of viscose rayon fibers were performed in the presence of 3 % phosphoric acid and 4 % boric acid (PA–BA) impregnation. The results showed that PA–BA impregnation enhanced thermal stability and prevented the evolution of volatile by-products. During the oxidation stage carried out at 250 °C, the cellulose II crystalline structure was totally lost due to the decrystallization process. Carbonization was carried out in a pure nitrogen atmosphere at temperatures ranging from 600 to 1000 °C. The results obtained from the fiber thickness, linear density, carbon fiber yield, elemental analysis, volume density, X-ray diffraction, infrared (IR) and Raman spectroscopy, tensile testing, and electrical conductivity measurements showed that the carbonization temperature had a significant effect on the structure and properties of the resulting carbon fibers. Carbon fibers obtained from the oxidized viscose rayon fibers showed physical and chemical transformations with increasing carbonization temperature and were characterized by a reduction in fiber thickness and linear density values due to the removal of non-carbon elements together with increases in the carbon content, carbon to hydrogen ratio (C/H), volume density, tensile strength, tensile modulus, and electrical conductivity values. X-ray diffraction analysis showed that the interplanar d-spacing (d ₀₀₂) decreased, and that the apparent crystallite thickness (L _c) and the apparent crystallite width (L _a) increased with increasing temperature. IR spectroscopy in agreement with the elemental analysis showed the total loss of OH, CH, C=O, CH₂, C–O, and C–O–C groups arising from the completion of dehydration and dehydrogenation reactions indicating total elimination of the cellulose structure and the formation of amorphous carbon during high temperature treatment.     

剑麻纤维素微晶的制备与表征

通过对剑麻纤维进行预处理、碱处理、酸解等步骤制备剑麻纤维素微晶,采用红外光谱(FT-IR)、X射线衍射(XRD)、偏光显微镜(POM)、扫描电镜(SEM)、差示扫描量热(DSC)和热重分析(TGA)等方法对产物进行了表征。红外谱图分析表明,所制备的剑麻纤维素微晶的主要成分为纤维素;而XRD、POM和SEM结果表明,剑麻纤维素微晶以纤维素Ⅰ的形式存在,长度尺寸在50μm~150μm之间,直径10μm左右;DSC和TGA热分析结果表明,剑麻纤维素微晶在323.7℃处有一尖锐的结晶熔融吸热峰,其初始热分解温度达到337℃,比普通剑麻纤维的初始热分解温度提高60℃,并且其在700℃时的最后残留物仅为0.05%。     

热致液晶聚酰胺与尼龙66相容原位复合材料研究

合成了半柔性热致液晶聚酰胺(TLCPa),通过熔融共混方法制备了TLCPa/PA66共混物.用差示扫描量热(DSC)、广角X射线衍射(WAXD)、扫描电子显微镜(SEM)和傅里叶红外光谱(FTIR)等分析手段对共混物进行了综合研究.DSC研究表明:TLCPa的加入使共混物的熔融温度和结晶温度向低温方向漂移,结晶速率下降.根据WAXD分析:强剪切有利于TLCPa与PA66分子间形成氢键作用,TLCPa与PA66形成共晶.SEM分析显示:TLCPa与PA66具有良好的相容性,沿流动方向TLCPa变形成为微纤.FTIR分析显示TLCPa与PA66分子间存在氢键作用.     

Determination of molecular orientation of uniaxially stretched polyamide fibers by polarized infrared spectroscopy: comparison of X-ray diffraction and birefringence methods

Polarized infrared (IR) spectroscopy has been used to determine the crystalline and amorphous orientation of polyamide fibers. The transition moment angle of the band at 936 cm-1 of PA66 was determined to be 48 degrees using IR spectroscopy and birefringence measurement. The crystalline orientation of PA66 fibers was estimated from the band at 936 cm-1 while the amorphous orientation of PA66 fibers was obtained by an indirect method. The alpha crystalline orientation of PA6 has been obtained using the band at 930 cm-1 and the amorphous orientation of PA6 has been determined using the band at 1124 cm-1. Crystalline orientation increased rapidly at low draw ratios (DR<3) and increased slowly at higher draw ratios (DR>3) for both PA66 and PA6 fibers, while the amorphous orientation increased slowly throughout the whole extension range for PA66 fibers. A good correlation was found between the crystalline orientation values obtained by infrared spectroscopy and other methods such as X-ray diffraction for PA66 and PA6 fibers. On the basis of this observation, it has been concluded that polarized infrared spectroscopy can be used reliably to measure the orientation of polyamide fibers without combining with other techniques.     

乙酰乙基纤维素的热致液晶性能及其与PA6原位复合的研究

将乙基纤维素乙酰化制备乙酰乙基纤维素。用ＮＭＲ，ＩＲ测定了ＡＥＣ的乙酰取代度，用ＤＳＣ，ＨＳＰＬＭ研究了ＡＥＣ的热致液晶性能，织构与Ａ－ＤＳ的关系。在此基础上研究了ＰＡ６／ＡＥＣ原位复合单丝的形态结构和力学性能，证明一定条件下ＡＥＣ对ＰＡ６有明显增强作用，总取代度增大是主要作用机制。     

含联苯基和亚胺基热致性聚酯液晶的合成与表征

以N,N′-二(ω-羟乙基)苯均四甲酰二亚胺(BHDI)、对苯二甲酰氯(TPC)、4,4′-二(β-羟己氧基)联苯(BP6)为单体,通过改变BHDI和BP6的物质的量比,制备了三种主链上同时含有联苯基和亚胺基的聚酯液晶(PBHT)。采用傅里叶红外光谱(FT-IR)、差示扫描量热分析仪(DSC)、偏光显微镜(POM)、广角X射线衍射(WAXD)及热重分析(TGA)等手段对聚合物结构及性能进行表征。结果表明,当BP6和BHDI物质的量比为4∶3时,聚酯液晶(PBHT)的液晶区间最宽,为116℃-190℃;该类液晶在液晶态温度区间呈现出向列型液晶丝状织构,WAXD分析显示为半结晶性聚合物;随着BHDI含量的增大,液晶聚酯热性能有所提高。     

纳米SiO_2/PVA杂化材料纸张表面增强剂的制备及性能

以正硅酸乙酯(TEOS),γ-氨丙基三甲氧基硅烷(KH-550)和聚乙烯醇(PVA)为主要原料,基于溶胶-凝胶(sol-gel)工艺,制备了一种纳米SiO2/PVA杂化材料,并将其用于纸张表面增强。通过红外光谱(IR),X射线衍射(XRD),差示扫描量热(DSC)和热重分析(TGA)对杂化材料进行表征,结果表明,纳米SiO2和PVA之间产生了化学键的结合,无机相的引入使杂化材料的热分解温度升高,结晶度降低。初步应用实验结果表明,当增强剂用量为1%时,纸张的环压指数提高27%,拉伸强度提高40%,撕裂度提高33%,拉毛强度提高35%。     

Multi-walled carbon nanotubes and poly(lactic acid) nanocomposite fibrous membranes prepared by solution blow spinning

Nanocomposite fibers based on multi-walled carbon nanotubes (MWCNT) and poly(lactic acid) (PLA) were prepared by solution blow spinning (SBS). Fiber morphology was characterized by scanning electron microscopy (SEM) and optical microscopy (OM). Electrical, thermal, surface and crystalline properties of the spun fibers were evaluated, respectively, by conductivity measurements (4-point probe), thermogravimetric analyses (TGA), differential scanning calorimetry (DSC), contact angle and X-ray diffraction (XRD). OM analysis of the spun mats showed a poor dispersion of MWCNT in the matrix, however dispersion in solution was increased during spinning where droplets of PLA in solution loaded with MWCNT were pulled by the pressure drop at the nozzle, producing PLA fibers filled with MWCNT. Good electrical conductivity and hydrophobicity can be achieved at low carbon nanotube contents. When only 1 wt% MWCNT was added to low-crystalline PLA, surface conductivity of the composites increased from 5 x 10(-8) to 0.46 S/cm. Addition of MWCNT can slightly influence the degree of crystallinity of PLA fibers as studied by XRD and DSC. Thermogravimetric analyses showed that MWCNT loading can decrease the onset degradation temperature of the composites which was attributed to the catalytic effect of metallic residues in MWCNT. Moreover, it was demonstrated that hydrophilicity slightly increased with an increase in MWCNT content. These results show that solution blow spinning can also be used to produce nanocomposite fibers with many potential applications such as in sensors and biosensors.     

超声波预处理对速生材木浆纤维结构的影响

利用扫描电镜、Ｘ－射线衍射、傅利叶变换红外光谱等现代测试分析手段,探讨了超声波处理马尾松、尾叶按两种速生材木浆纤维过程中,形态结构、超微结构、超分子结构、对试剂可及度的变化。结果表明,超声处理后木浆纤维壁出现裂纹、细胞壁发生位移和变形、有更多的次性壁中层（Ｓ２）暴露出来,处理后的木浆纤维仍保持原有的纤维素晶型和两相共存的微细结构,晶粒尺寸的基本不变。结晶变化与超声处理的条件有关,超声波处理后,纤维     

Modification of properties of rayon fibre by graft copolymerization with acrylic monomers

The change in rayon fibre properties due the grafting polymerization of methyl metacrylate (MMA) and butyl acrylate (BA) was investigated. The formation of rayon-g-PMMA or PBA was confirmed by FTIR spectroscopy, X-ray analysis, and TGA. The adhesion to PMMA and epoxy resin matrixes was determined using the microdrop technique. The PBA or PMMA grafting on the fibre led to lower mechanical properties than the ungrafted rayon fibre. However, the grafted rayon had better thermal properties than the ungrafted rayon and a shift of the decomposition temperature of the rayon was observed. The PMMA grafted to rayon improved the interfacial adhesion when PMMA was used as matrix (microdrop technique). The grafted polymer (PBA or PMMA) restricted the “wetting” of the fibre when epoxy resin was used as matrix and lowering the adhesion in comparison with ungrafted rayon fibre.     

Formation studies of TiC from carbon coated TiO2

This paper deals with the formation of titanium carbide from carbon coated titanium dioxide precursors. This study makes use of differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction (XRD), and both scanning and transmission electron microscopy (SEM and TEM). DSC curves of both coated and mixed 33.2 wt % carbon containing titania demonstrates the superiority of the coated precursor by exhibiting both more reactions and reactions at lower temperatures than the mixed powder. Weight loss as powders were reacted in argon at varying temperatures was measured using TGA, while heat flow vs. temperature was measured by DSC. The weight loss allowed for calculation of the activation energy of TiC via the formation of various lower oxides of titanium. The activation energy was calculated as 731.6 ± 24.2 kJ/mol. XRD was used to characterize the products resulting from the reaction of the carbon coated precursor at isotherms at each 100 °C interval from 1100 to 1500 °C, inclusive. These diffraction patterns support the hypothesis that the TiC formation proceeds through the formation of lower oxidation states of titanium.     

液晶聚合物对PA1010/滑石粉杂化材料增容作用的研究

用液晶聚合物（LCP）作增容剂，采用熔融插层法制备了PA1010／滑石粉（FCP）杂化材料，用广角X射线衍射，小角X射线散射，DSC和TGA研究了液晶聚合物对杂化材料的结构，结晶行为和热稳定性的影响，结果表明，LCP的增容使用使PA1010／FCP杂化材料挤出时的粘度显著下降，从而降低加工温度5℃左右，当LCP质量分数为3％，9％时对应杂化材料H3，H9中滑石粉的层间距扩展为40．1nm和25．2nm，LCP的增容作用使PA1010能插层于滑石粉片层间，而其结晶行为基本未受影响，杂化材料的热稳定性良好。     

Preparation and characterization of a novel bone graft composite containing bone ash and egg shell powder

Egg shells which were hitherto discarded as wastes were collected, purified and powdered into a particle size in the range of 5–50 μm. A composite bone graft material in cylindrical form was prepared using egg shell powder (ESP), bone ash (BA) and gelatin. These bone grafts were characterized for their FT–IR, TGA, XRD, SEM and mechanical properties. The mechanical studies indicate that the composite having a stoichiometric ratio of BA (3 g) and ESP (7 g) has shown better mechanical properties. X-ray diffraction (XRD) data indicated the crystallographic nature of BA is akin to hydroxyapatite (HA) and both BA and ESP did not lose their crystalline nature when bone grafts were prepared. This revealed that ESP may be used as a component in bone graft utilizing the solid waste from the poultry industry.     

粘胶纤维与Lyocell纤维增强聚乳酸复合材料的性能比较

以聚乳酸(PLA)为基体,分别采用粘胶纤维与Lyocell纤维这2种典型的再生纤维素纤维为增强纤维,通过熔融共混和注塑成型制备了再生纤维素纤维/PLA复合材料,并对这2种复合材料的性能进行了比较研究。结果表明,采用粘胶纤维或Lyocell纤维增强均可有效提高PLA复合材料的结晶度、力学性能和维卡软化温度。粘胶纤维的锯齿形截面有利于其与PLA基体的结合,因此粘胶纤维/PLA复合材料具有略高的冲击强度及拉伸强度。Lyocell纤维增强更有利于复合材料结晶度的提高,使得Lyocell/PLA复合材料具有更高的弹性模量和维卡软化温度。     

一种低支化聚酯液晶的合成及性能表征

采用不同比例的4,4′-对苯二甲酰二羟苯甲酸乙二醇酯（TOBB）与偏苯三酸酐（TMA）反应,合成端基含有羧基的哑铃型聚酯液晶和低支化度的聚酯液晶。通过红外光谱（FT-IR）、差示扫描量热（DSC）、偏光显微镜（POM）、广角X射线衍射（WAXD）及热重分析（TGA）等对其结构及性能进行表征。结果表明,所合成的聚酯液晶呈...     

Synthesis and physicochemical properties of cobalt aluminium hydrotalcites

Cobalt aluminium hydrotalcites with different compositions were prepared by a coprecipitation method under low supersaturation conditions. The compounds were characterized by X-ray diffraction (XRD), infrared absorption (IR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and BET surface area measurements. XRD and IR studies revealed that all the compounds are single-phase crystallized under a hydrotalcite-like network. Hydrothermal treatments given to the aged sample increased the crystallinity of the samples. TG studies showed two stages of weight loss, the first due to the removal of interlayer water and the second ascribed to the removal of water molecules from the brucite sheet and CO₂ from the interlayer carbonate anion, whose transition temperature depends on the Co/Al atomic ratio. Thermal calcination of these materials results in the formation of high surface area non-stoichiometric spinel phase whose crystallinity increases with increase in the calcination temperature attributed to the sintering of the particles.     

SiBN三元陶瓷纤维的聚硼硅氮烷裂解转化制备和性能

以三氯硅烷、六甲基二硅氮烷、三氯化硼和甲胺为原料合成聚硼硅氮烷前驱体,对前驱体进行熔融纺丝和不熔化处理,将其高温裂解后制备出SiBN陶瓷纤维。使用FT-IR、NMR、XRD、TEM、TGA等表征手段研究了在不同聚合温度下聚硼硅氮烷前驱体的化学结构特征、SiBN陶瓷纤维的高温热稳定性、介电性能以及力学性能。结果表明：在不同温度下制备的聚硼硅氮烷前驱体的骨架为Si-N-B,均含有HSiN₃、BN₃及NCH₃等结构。在1400℃热处理后SiBN陶瓷纤维仍保持无定形态,直径为14 μm,拉伸强度达到0.91 GPa。在氮气气氛中SiBN陶瓷纤维从室温到1400℃的失重为1.5%,表明这种纤维具有较高的热稳定性。SiBN陶瓷纤维的介电常数为2.6~2.8,损耗角正切的数量级为10^-2。     

Sol–gel synthesis and spark plasma sintering of Ba0.5Sr0.5TiO3

Ultrafine Ba_0.5Sr_0.5TiO₃ powders were prepared by using barium nitrate, strontium nitrate, tetrabutyl titanate, and ammonia via citrate–nitrate combustion process at low temperature (500 °C), along with the X-ray diffraction (XRD), differential scanning calorimetry (DSC)/thermogravimetry analysis (TGA) and scanning electron microscopy (SEM) analytic reports. Spark plasma sintering was carried out to obtain the ultrafine crystalline BST and to improve the dielectric properity. It was found that the sintered BST showed ultrafine crystalline microstructure. At 25 °C, the dielectric constant and dissipation factor of the sintered sample were 1533 and 0.0063 at 10 kHz.     

PAN纤维热松弛行为控制与聚集态结构调控EI北大核心CSCD

聚丙烯腈(PAN)纤维在纺丝过程中会形成受迫高弹形变,在受热条件下会出现物理收缩为代表的热松弛行为,发生解取向。通过热力学分析仪(TMA),动态力学分析仪(DMA),广角X射线衍射法(WAXD)等手段研究PAN纤维的热松弛行为,并且通过张力和温度对其进行控制。结果表明:PAN纤维纺丝过程形成的高弹形变约占10%以上,在高温下会迅速回复发生解取向。通过施加适当的张力和提高温度可以在不损失取向结构的同时将高弹形变转化为塑性形变。在张力和温度的作用下,纤维内部聚集态结构重排,分子链取向进一步提高,晶态结构进一步完善,纤维尺寸稳定性提高50%以上。研究表明经此方法处理的碳纤维微晶沿分子链排列更加规整,性能得到了有效提升。     

Growth,characterization and dielectric property studies of gel grown barium succinate single crystals

. Single crystals of barium succinate (BaC4H4O4) were grown in silica gel medium using controlled chemical reaction method. Plate-like single crystals of size up to 3 × 2 × 0·2 mm³ was obtained. Single crystal X-ray diffraction (XRD) studies confirmed that structure of the title compound is tetragonal. Powder X-ray diffraction (PXRD) pattern of the grown crystal and the Fourier transform infrared (FT–IR) spectrum in the range 400–4000 cm^–1 are recorded. The vibrational bands corresponding to different functional groups are assigned. Thermal stability of the grown crystals is confirmed by differential scanning calorimetry (DSC). Dielectric constant and dielectric loss have been calculated and discussed as a function of frequency at different temperatures.