Nd10.5Pr2.5Fe80Nb1B6非晶快淬薄带等温晶化行为及矫顽力研究

研究了Nd10.5Pr2.5Fe80Nb1B6非晶快淬薄带在943,973和1003 K等温晶化与薄带组织和矫顽力的关系.结果表明,Nd10.5Pr2.5Fe80Nb1B6快淬薄带在943 K等温晶化所需晶化孕育时间为12 min,973 K时为5Inin,而1003 K时不足5lIlin.Ndl 0_5%,‰NbB6在1003K晶化25 min后所得的(Nd,Pr)2Fe14B平均晶粒尺寸为163 nm,添加Nb显著延缓了Nd10.5Pr2.5Fe80Nb1B6快淬薄带晶化后的晶粒尺寸长大.加Nb,Pr能有效提高Nd10.5Pr2.5Fe80Nb1B6的矫顽力.在973 K晶化处理19min时得到平均晶粒尺寸为96 nm的(Nd,Pr)2Fe14B单相组织,其最大矫顽力为1616 kA·m-1.     

Nd10.1Fe(83.7-x-y)CoxZryB6.2永磁材料结构和磁性能的研究

采用熔体快淬及晶化热处理工艺制备Nd10.1Fe(83.7-x-y)CoxZryB6.2纳米晶永磁材料. 在快淬速度为18 m·s-1时, 经710 ℃/4 min晶化处理后, Nd10.1Fe76Co5Zr2.7B6.2粘结磁体出现最佳磁性能, 分别为Br=0.67 T, JHc=754 kA·m-1, (BH)max=75.1 kJ·m-3. 粘结磁体的磁性能对于快淬速度非常敏感. 随着合金元素的添加, 出现最佳磁性能的快淬速度逐渐减少. 为了得到最佳磁性能, 除了选择合适的快淬速度外, 添加合适的合金元素变得非常重要.添加Zr元素抑制了亚稳相的析出以及细化了晶粒尺寸.比较不加Zr元素的Nd10.1Fe78.7Co5B6.2, 添加Zr元素晶化温度增加了9 ℃, 表明Zr元素也增加了快淬薄带的热稳定性.     

铌和锆对(Nd,Pr)2Fe14B/α-Fe快淬合金晶化和磁性能的影响

研究了Nb和Zr添加对快淬纳米双相(Nd,Pr)2Fe14B/α-Fe合金晶化行为和磁性能的影响. 结果表明 (Nd0.4Pr0.6)8.5Fe85.5B6合金非晶晶化时, 在α-Fe相初始晶化后, 出现了(Nd,Pr)3Fe62B14亚稳相, 最终亚稳相分解形成(Nd,Pr)2Fe14B和α-Fe两相组织; (Nd0.4Pr0.6)8.5Fe84.5Nb0.5Zr0.5B6非晶晶化时, 同时析出α-Fe相和(Nd,Pr)2Fe14B相. 这说明添加Nb和Zr可避免亚稳相的形成并细化晶粒, 最大磁能积(BH)max从复合添加前的107.5上升到143.6 kJ·m-3. 而且, Nb和Zr原子在非晶晶化过程中可以部分取代Nd和Pr的晶位, 使稀土原子可以参与形成更多的硬磁相, 进一步提高了内禀矫顽力iHc. 合金(Nd0.4Pr0.6)8.5Fe84.5Zr0.5Nb0.5 B6经690 ℃退火10 min后磁性能最优, Br=1.10 T, iHc=534.2 kA·m-1, (BH)max=143.6 kJ·m-3.     

添加钛和碳对Nd9.4Fe79.6B11合金晶化方式、显微结构和磁性能的影响

研究了Ti和C添加对Nd9.4Fe79.6-xTixB11-yCy(x=0,1,2,4,6;y=0.5,1.5,3)合金晶化方式、显微结构和磁性能的影响规律。结果表明,适量Ti和C添加改变了合金的晶化方式,使-αFe相和Nd2Fe14B相同时从Nd9.4Fe75.6Ti4B10.5C0.5非晶基体中析出,避免了先析出相晶粒的长大,利于获得细小均匀的显微结构。适量Ti和C添加的Nd-Fe-B-Ti-C非晶合金在退火过程中易析出细小弥散的TiC和TiB2相,可作为形核质点促进形核,且可抑制晶粒长大,最终形成细小均匀的显微结构。综合性能较佳的Nd9.4Fe75.6Ti4B10.5C0.5合金退磁曲线具有优异的方形度,最佳退火条件下合金薄带的剩磁Br为0.91 T,矫顽力iHc为976 kA.m-1,磁能积(BH)max达135 kJ.m-3。文章最后对Ti和C添加合金微结构的形成机制进行了探讨。     

铜模吸铸Nd9Fe83-xTi4C4Bx（x=1015）合金组织演化和磁性能的研究

采用铜模吸铸及随后的退火处理制备了厚度为0.8 mm,成分为Nd9Fe83-xTi4C4Bx(x=10~15)的Nd2Fe14B/Fe3B型纳米复相磁体,对其组织演变和磁性能进行了研究。结果表明:在铸态合金中,x=10的合金微观组织主要由Nd2Fe14B,Fe3B,α-Fe和TiC相构成。而x=11~15的合金中除含上述各相外,还出现了Nd2Fe23B3相、未知相和非晶相,且随着B含量的增加,它们在合金中的相对含量有不同程度的增加;退火过程中,随着合金中亚稳相和非晶相的转化,Nd2Fe14B,Fe3B和α-Fe相对含量增加,但不同B含量合金的相结构变化差异明显,导致退火后磁体具有不同的磁性能。其中,x=12的合金在680℃退火5 min后获得了最佳磁性能:Br=0.63 T,iHc=98.12 kA·m-1,(BH)max=22.79 kJ·m-3。     

添加铌对铜模吸铸Nd9Fe81-x-yTi4C2BxNby（x=11,13,15;y=0,4）合金铸态组织及其晶化行为的影响

采用铜模吸铸制备了厚度为0.8 mm,成分为Nd9Fe81-x-yTi4C2BxNby(x=11,13,15;y=0,4)的Nd2Fe14B/Fe3B型纳米复合永磁合金块体样品,研究了添加Nb对合金铸态组织及其晶化行为的影响,并测试了其磁性能。结果表明:在合金中添加4%(原子分数)Nb元素,不仅能抑制吸铸样品表面Nd2Fe23B3软磁性相、Nd1.1Fe4B4非磁性相和未知相的形成,导致Nd2Fe14B,Fe3B和α-Fe相的相对量增加,而且促使样品内部在非晶基体上形成了少量的Nd2Fe14B和α-Fe,Fe3B纳米晶。添加了Nb的合金吸铸样品表现出一定的硬磁性,其中Nd9Fe66Ti4C2B15Nb4吸铸样品具有最高的矫顽力(Hci=116.66 k A·m-1);添加4%(原子分数)Nb使得合金在晶化过程中由原来的异相同温一步晶化转变为两步晶化,且初始晶化温度Tx均明显降低,两个放热峰的ΔTpx均增大。     

镨元素对(Nd,Pr)10.5(FeCoZr)83.5B6合金显微结构和磁性能的影响

研究了稀土元素Pr对快淬(Nd1-xPrx)10.5(FeCoZr)83.5B6(x=0,0.2,0.4,0.6,0.8,1.0)合金显微组织结构和粘结磁体磁性能的影响。通过部分过快淬获得由非晶和微晶共同组成的条屑,在实验优化的退火条件下晶化处理后,制备出最佳磁性能的系列粘结磁体。随Pr含量的增加,磁体的内禀矫顽力Hci单调上升,剩磁Br单调下降,(BH)m在x=0.6～0.8处达到最大值70.6kJ·m-3。Pr元素使合金非晶态的晶化转变温度和转化能降低,合金的显微组织结构变得较粗大和较不均匀,从而使快淬粘结磁体剩磁降低,但Pr2Fe14B化合物较高的磁晶各向异性场使磁体的内禀矫顽力提高。     

制备工艺对Pr2Fe14B/α-Fe纳米复合永磁材料组织与磁性的影响

用XRD,TEM和VSM等方法研究了快淬法制备的Pr2Fe14B/α Fe纳米复合永磁薄带的显微结构与磁性。比较了直接快淬和非晶晶化两种制备工艺对合金薄带显微结构和磁性能的影响。通过对Pr8Dy1Fe74.5Co10Nb0.5B6合金薄带高压退火,获得了Br=1.11T,Hci=816.0kA·m-1和(BH)max=188.8kJ·m-3的高性能。     

锆对纳米复相粘结磁体的组织结构和磁性能的影响

采用快淬、热处理及模压成形工艺,制备了成分为Nd10.5Fe78.4-xCo5ZrxB6.1(x=0,1.0,1.5,2.0,2.5)的5种粘结永磁体.采用XRD,DTA,AFM等方法对合金的组织结构、晶化行为进行了研究.结果表明:Zr含量的增加可提高材料的非晶形成能力;当Zr添加到一定量时,形成高熔点的Fe2Zr相,产生细化晶粒的作用;添加Zr元素显著地提高了合金的矫顽力,改善了退磁曲线矩形度,从而提高了最大磁能积.Nd10.5Fe78.4-xCo5ZrxB6.1永磁体在x=2时获得最佳磁性能,Br=0.659 T,Hcj=628KA·m-1,Hcb=419KA·m-1,(BH)m=73KJ·m-3.     

单辊快淬法制备高性能各向异性Nd_2Fe_(14)B/α-Fe纳米复相永磁材料

采用熔体快淬工艺制备了成分为Nd-Fe-B-P和Nd-Fe-B-P-Zr快淬带,组织结构研究和磁性能研究表明:添加P元素有利于Nd2Fe14B相晶粒沿C轴择优取向,形成(00L)织构;(00L)织构的形成使材料产生各向异性,沿垂直带面方向:Hci=495 k A·m-1,Jr=1.18T,(BH)max=190 k J·m-3。进一步添加元素Zr虽然有利于晶粒细化,但却抑制了织构的形成,得到的合金条带为各向同性磁体。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。