Optimal Conditions for Preparing Ultra-Fine CeO_2 Powders in A Submerged Circulative Impinging Stream Reactor

Cerium carbonate powders were produced in a submerged circulation impinging stream reactor （SCISR） from Ce（NO3）3· 6H2O. NH4HCO3 was used as a precipitant in the reaction. Cerium carbonate powders were roasted to produce ultra-fine cerium dioxide （CeO2） powders. The optimal conditions of such production process were obtained by orthogonal and one-factor experiments. The results showed that ultra-fine and narrowly distributed cerium carbonate powders were produced under the optimal flowing conditions. The concentrations of Ce（NO3）3 and NH4HCO3 solutions were 02,5 and 0.3 mol · L^-1, respectively. The concentration of PEG4000 added in these two solutions was 4 g · L^-1. The stirring ratio, reaction temperature, feeding time, solution pH, reaction time and digestion time were 900 r · min^- 1,80 ℃, 20 min, 5 - 6, 5 min and 1 h, respectively. The final product, CeO2 powders, was obtained by roasting the produced cerium carbonate in air for 3 h at 500 ℃. The finally produced CeO2 powders were torispherical particles with a narrow size distribution of 0.8 -2.5 μm. The crystal structure of CeO2 powders belonged to cubic crystal system and its space point 5 group was OH^5-FM3M. Under optimal conditions, powders produced by SCISR were finer and more narrowly distributed than that by Stirred Tank Reactor （STR）.

DYNAMIC RHEOLOGICAL BEHAVIOR OF POLYPROPYLENE FILLED WITH ULTRA-FINE POWDERED RUBBER PARTICLES

Dynamic rheological characteristics of polypropylene (PP) filled with ultra-fine full-vulcanized powdered rubber (UFPR) composed of styrene-butadiene copolymer were studied through dynamic rheological measurements on an Advanced Rheometric Expansion System (ARES). A specific viscoelastic phenomenon, i.e. 'the second plateau', appeared at low frequencies, and exhibits a certain dependence on the amount of rubber particles and the dispersion state in the matrix. This phenomenon is attributed to the formation of aggregation structure of rubber particles. The analyses of Cole-Cole diagrams of the dynamic viscoelastic functions suggest that the heterogeneity of the composites is enhanced on increasing both particle content and temperature.

Hydrogen Reduction:A Novel Method of Synthesizing Ultra-fine Chromic Oxide Powder

The ultra-fine chromic oxide powder was prepared by a novel gas-solid reduction reaction.Na2CrO4 was firstly reduced with hydrogen at 400-600 ℃.The obtained reduction products,mainly the mixture of NaCrO2 and sodium hydroxide（NaOH）,were converted into chromic oxide through hydrolysis followed by calcination.The obtained chromic oxide product was characterized by powder X-ray diffraction（XRD） and SEM.The results show that the hydrolysis process of sodium chromite is the key step and lower reduction temperature helps intensify the hydrolysis process.

Strengthening of HT250 by modified ultra-fine ceramic powders

In this study, three kinds of modified ultra-fine ceramic powders marked A, B and C, which were prepared by each of three different modifiers mixing with a commercial SiC, were added to HT250 cast iron, respectively, and the effects of the modified ultra-fine ceramic powders on microstructure, mechanical properties and wear resistance were studied. Metallographic examination, tensile test, scanning electron microscopy, and three-dimensional surface topography were applied to analyze and compare the samples containing modified powder with the original samples. The results showed that the most obvious modification effect among the powders was seen in the sample containing powder A, with the graphite and eutectic cells being refined, the tensile strength being increased by 36.9%, and the wear resistance being improved by 45.5% and 47.2% under loads of 150 N and 300 N, respectively. The improvements of mechanical properties and wear resistance in the HT250 cast iron with the modified ultra-fine ceramic powders were attributed to the synergistic effect of the grain refinement with the powder acting as a hard particle phase and the lubrication by the graphite.

Preparation and study on performance of submicron nickel powder for multilayer chip positive temperature coefficient resistance

Base metal nickel is often used as the inner electrode in multilayer chip positive temperature coefficient resistance （PTCR）. The fine grain of ceramic powders and base metal nickel are necessary. This paper uses reducing hydrazine to gain submicron nickel powder whose diameter was 200-300 nm through adjusting the consumption of nucleating agent PVP properly. The submicron nickel powder could disperse well and was fit for co--fired of multilayer chip PTCR. It analyes the submicron nickel powder through x-ray Diffraction （XRD） and calculates the diameter of nickel by PDF cards. Using XRD analyses it obtains several conclusions： If the molar ratio of hydrazine hydrate and nickel sulfate is kept to be a constant, when enlarging the molar ratio of NaOH/Ni^2＋, the diameter of nickel powder would become smaller. When the temperature in the experiment raises to 70-80 ℃, nickel powder becomes smaller too. And if the molar ratio of NaOH/Ni2＋ is 4, when molar ratio of （C2H5O）2/Ni^2＋ increases, the diameter of nickel would reduce. Results from viewing the powders by optical microscope should be the fact that the electrode made by submicron nickel powder has a better formation and compactness. Furthermore, the sheet resistance testing shows that the electrode made by submicron nickel is smaller than that made by micron nickel.

PREPARATION OF ULTRAFINE NICKEL POWDER

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Preparation of Well Dispersed and Ultra-Fine Ce(Zr)O_2 Mixed Oxide by Mechanochemical Processing

Ultra-fine CeO_2-ZrO_2 mixed oxide was successfully synthesized by wet-solid phase mechanochemical processing, Ce_2(CO_3)_3·8H_2O, ZrOCl_2·xH_2O and ammonia were used as reactants. It is found that the crystalline Ce_2(CO_3)_3·8H_2O and ZrOCl_2·xH_2O are changed to amorphous cerium and zirconium hydroxide precursor after milling with ammonia, and Ce_(0.15)Zr_(0.85)O_2 mixed oxide with pure tetragonal phase structure and medium particle size(D_(50))less than 1μm is formed by calcining precursor over 673 K. The XRD patterns indicate that the crystal unite size increases with rising calcining temperature due to crystal growth. However, the particle size and BET surface area of the Ce(Zr)O_2 mixed oxide decreases with rising calcining temperature, which may be attributed to the contract of particles and the vanish of holes inside grains.

Preparation of fine nickel powders via reduction of nickel hydrazine complex precursors

Fine nickel(Ni) powders with controllable particle sizes were synthesized via the reduction of nickel hydrazine complex precursors of pure [Ni(N2H4)2]Cl2 and a mixture of [Ni(N2H4)2]Cl2 and [Ni(N2H4)3]Cl2 in aqueous solution. The mechanism of the formation of metallic Ni powders experiences the reduction of nickel hydroxide by hydrazine released from the ligand exchange reaction between nickel hydrazine complex and NaOH. In comparison with the method of preparing Ni powders from nickel salts,the method of making Ni powders via the reduction of nickel hydrazine complex precursors shows the advantages of using half dosage of hydrazine for complete reduction of nickel ions in solution,and the obtained Ni particles show less agglomeration and better dispersibility. Moreover,the average particle size of nickel powders can be controlled from 180 to 260 nm by adjusting the reaction molar ratio and concentration.

Preparation of ultrafine nickel powder by wet chemical process

The main technical problems of nickel powder for multiplayer ceramic capacitors are particle size controlling, the agglomeration and tap density. Ultrafine nickel powders with submicron size and spherical shape were synthesized by the hydrazine reduction of nickel sulfate in ethanol-water solvent. The effects of reaction temperature, nucleator and flow rate of nickel sulfate solution on nickel powders properties were investigated. The nickel particles synthesized were characterized by SEM and TGA. The results show that the average particle size changes from 0.1 to 0.7 μm by adjusting reaction temperature (53- 73 ℃) and flow rate of nickel sulfate solution (50- 100 mL/min). Moreover, temperature below 60 ℃ and appropriate flow rate of nickel sulfate solution (85 mL/min) are in favor of obtaining particles with high tap density (>3.0 g/cm3). In addition, the introduction of nucleator is useful to obtaining particles with narrow size distribution.

Effects of Fe additive on diamond crystallization from carbonyl nickel powders-C system under HPHT condition

In this paper, diamond crystallization from carbonyl nickel powders-C and carbonyl nickel powders + Fe–C systems are investigated in detail at a pressure of 6.0 GPa and temperatures ranging from 1410°C–to 1435°C by temperature gradient growth. The effects of Fe additive on the crystal morphology are discussed in the diamond crystallization process.Furthermore, Fourier infrared measurement results indicate that the spectrum of the diamond obtained from Ni + Fe–C system after annealing treatment is nearly consistent with that of natural diamond crystal. We believe that this study is of benefit to a further understanding of the growth mechanism of natural diamond.

Producing High Purity Nickel Metal Powder from Nickel Wastes through Acidic Leaching by Sulfuric Acid

Nickel has found increasing application in electronic,automobile manufacturing,plating,and metal industries and so on.Producing high quality metal powders to satisfy increasing demand for advanced materials is of very high importance.There are a few numbers of standard powder production techniques.An acidic leaching has been applied in present research.Sulfuric acid has been used to leach nickel wastes of plating industry.To produce nickel oxide powder furnaces with no protecting atmosphere and to produce pure nickel powder,tube furnace with hydrogen atmosphere has been applied.Variables performed in the research are time,density of sulfuric acid,and amount of hydrogen peroxide.To analyze powders produced,EDS element analysis and to determine size of powder particles,SEM has been applied.It was shown by the results that the highest amount of nickel dissolution in sulfuric acid(98%)has taken place during one hour and there is a direct relationship between hydrogen peroxide amount and nickel dissolution in sulfuric acid.

线锯用金刚石微粉表面化学镀镍工艺及性能研究

金刚石微粉性能是提升金刚石线锯性能的关键因素。用化学镀方法在线锯用金刚石微粉表面镀镍,通过正交试验研究金刚石粒度、次亚磷酸钠浓度、镀液pH值和镀液温度对化学镀镀层沉积速率、镀层密度、镀层耐腐蚀性能、镀层致密度等性能的影响。结果表明:M1/2、M6/12、M20/30三种不同粒度金刚石微粉,在次亚磷酸钠浓度为25~35g/L、化学镀液pH值为3~11、化学镀温度为30℃~90℃时,针对镀层沉积速率、镀层密度和镀层耐腐蚀性的最佳工艺参数不同;不同粒度的金刚石微粉在相同工艺条件下化学镀镍,金刚石微粉粒度越大,镀层越均匀致密;金刚石微粉化学镀镍各工艺参数之间相互作用,共同影响镀层性能。对于不同粒度的金刚石微粉,各因素对镀层性能的影响权重不同,因此针对不同粒度、不同镀层性能需求的金刚石微粉应采取不同的镀覆工艺参数。

NaFeS_(2)强化褐铁矿型红土镍矿固态还原富集镍钴的研究

以NaFeS_(2)为添加剂,研究了NaFeS_(2)用量对红土镍矿固态还原-磁选富集镍、钴及红土镍矿还原行为的影响。结果表明,随着NaFeS_(2)添加量增加,还原过程红土镍矿的软熔特性温度相应降低,还原所得Ni-Co-Fe合金颗粒随之增大;添加10%NaFeS_(2)时,镍、钴的富集和回收效果好,红土镍矿经压团于1100℃还原60 min,再经磨矿-磁选可获得Ni、Co、Fe品位分别为7.89%、0.66%、74.01%,Ni、Co、Fe回收率分别为97.13%、86.78%、35.81%的优质镍钴铁粉产品。

玻璃粉改性Ni60复合涂层的制备及其摩擦磨损性能

采用火焰喷涂技术在45钢表面制备了Ni基合金/玻璃粉复合涂层,通过扫描电镜(SEM)、能谱分析(EDS)、X射线衍射(XRD)、显微硬度分析以及销-盘式摩擦磨损试验等方法,研究了玻璃粉添加量对Ni基合金涂层微观结构、物相组成、硬度及摩擦学性能的影响.结果表明:随着玻璃粉含量的增加,复合涂层的显微硬度值呈现先升高后降低的趋势,最高达到681 HV 0.2.复合涂层的摩擦系数和体积磨损率均呈现先降低后升高的趋势.10%玻璃粉添加量的复合涂层摩擦系数低至0.13,磨损率低至0.21×10^(-5) mm^(3)/(N·m).表明适量玻璃粉的添加有利于Ni基合金涂层摩擦学性能的改善.

镍粉/碳纤维复合导电沥青胶浆的电热性能

基于电阻率、升温速率、车辙因子和劲度模量等指标优选出镍粉/碳纤维复合导电沥青胶浆Ni-CF-2,研究了其电性能和热性能,并根据其内导电材料微观分布研究其导电机理。结果表明,Ni-CF-2在交流电下的电流值显著大于直流电,但非线性伏安特性离散性较大,且同时存在温敏效应和压敏效应;10 mm厚Ni-CF-2的导热系数比基质沥青高18.8%,通电时热量呈现层状的均匀分布,20 min内升温幅度达50℃以上,并具有良好切缝愈合能力;Ni-CF-2试样由导电颗粒的接触或电子跃迁形成导电通路。

Ni–MgO核–壳纳米粉体的制备

采用包覆热分解烧结法,制备了多层陶瓷电容器内部电极用MgO包覆Ni纳米粉体,讨论了反应物浓度和分散剂含量对包覆纳米镍盐前驱体颗粒大小和均匀性的影响,分析了还原烧结温度对包覆纳米Ni粉球形度和分散性的影响,并利用X射线衍射仪、扫描电镜、透射电镜、热机械分析仪对MgO包覆纳米Ni粉进行了表征分析。结果表明:反应物浓度达到足以引起反应爆炸成核时,能够获得纳米镍盐颗粒;添加适量的分散剂,可以得到分散良好的纳米镍盐前驱体颗粒;还原烧结温度700℃时,可以获得球形度和分散性良好的MgO包覆纳米Ni粉;MgO包覆在纳米Ni粉表面,形成了核壳结构,该纳米Ni粉具有良好的收缩延迟效果。

镍铁粉对水泥水化性能的影响

采用镍铁渣制成粒径小于0.075 mm的粉体,作为矿物掺合料取代部分水泥,研究镍铁粉不同掺量对水泥水化性能以及强度的影响。XRF分析发现,镍铁粉中含有较多的SiO_(2)、MgO、FeO,具有较高的火山灰活性。镍铁粉的掺入可以较大程度上延缓水泥水化时间,相较空白组,掺30%镍铁粉时,第2个水化放热峰的出现时间延缓8 h左右;降低体系的水化放热量,相较空白组,当镍铁粉掺量为10%、20%、30%时,体系的累计放热量依次下降33%、46%、63%;掺入镍铁粉明显降低试块的抗压强度,但镍铁粉具有二次水化作用,可以使试块后期抗压强度增幅较大,掺20%镍铁粉试块的28 d抗压强度可达到空白组的86%。

废旧锂电池极片热解试验研究

废旧锂电池作为一种二次资源,蕴藏巨大的回收价值。本文结合其主要成分热解性质,开展废旧锂电池极片的热解试验。废弃锂电池破碎分选后,正负极片热解过程的主要影响因素有温度、时间、真空度和气氛等。试验结果表明,热解温度为400℃,热解时间为0.75 h时,真空和氮气气氛可获得良好的热解效果,黑粉产率为75%~78%,镍、钴、锰等主要金属的回收率大于95%。

激光粒度仪湿法测定不同形貌超细镍粉平均粒度的研究

超细镍粉诸多物化性质随粉末形貌、粒径等参量的变化发生显著改变,因此针对超细镍粉的粒度的准确测定至关重要。确定激光粒度仪测定超细镍粉平均粒度的最佳测试条件,选用湿法测定方法,以多孔状、片状和球状超细镍粉对研究对象,研究了分散剂种类、超声时间、分散剂质量分数、遮光度及采样轮数等参数对超细镍粉平均粒径测定结果的影响。结果表明,在实验选用的6种分散剂FMES、L64、CAB、PECPM、CTAC和G-18中,添加FMES分散剂测得的超细镍粉D50值最小,而添加G-18分散剂测得的超细镍粉D50值最大,表明FMES分散剂改善了3种形貌的超细镍粉在水中的团聚,使粒度测量的准确性更高。当超声时间为8 min时,孔状超细镍粉测得的D50=4.403 μm,片状超细镍粉测得的D50=1.345 μm,球状超细镍粉测得的D50=1.289 μm。随着超声时间持续延长,3种形貌的超细镍粉测得的D50值逐渐趋于平稳,其中片状和球状形貌超细镍粉测得的D50值与电镜测试结果较为相符,而孔状超细镍粉D50值与电镜测试结果差别明显,表明激光粒度仪湿法测定不适用于孔状形貌的镍粉。采样轮数与粒度测试值具有强线性相关性,超声时间为8 min时,相邻两轮的测试结果更相近,从而确定了适宜的超声时间为8 min。综上所述,确定了片状和球状超细镍粉平均粒度的最佳测试条件为:超声时间8 min、分散剂FMES质量分数1.5%、遮光度10%—20%。在最佳测试条件下重复测试6次,片状和球状超细镍粉的平均粒度数据具有较高的准确性和重现性。

Preparation of high emissivity NiCr_2O_4 powders with a spinel structure by spray drying

Spray-drying was used to produce the high emissivity NiCr2O4 powders with a spinel structure. Preliminary investigations focused on fabricating the high emissivity powders for infrared radiation coatings and finding the relationship between microstructure and emissivity. The NiCr2O4 powders were characterized for composition, microstructure, and infrared emissivity by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, infrared radiant instrument, and Fourier transform infrared spectra （FT-IR）. Thermogravimetry and differential thermal analysis show that the appropriate baking temperature for NiCr2O4 powder preparation is about 1200？C. The emissivity measurement and FT-IR spectra show that, because of the special spinel structure, the NiCr2O4 powders have a high emissivity about 0.91. Spray-drying is a suitable method to produce the high emissivity ceramic powders.