双合金混粉法添加镝对烧结Nd-Fe-B磁体的磁性能及微观结构的影响

研究双合金混粉法添加Dy对烧结Nd-Fe-B磁体的磁性能和微观结构的影响。结果表明:添加少量Dy能够同时提高磁体的矫顽力和最大磁能积;当Dy含量为1.0%时,磁体的最大磁能积达到最大值。烧结温度从1065℃增加到1085℃时,烧结Nd-Fe-B磁体的磁性能没有急剧恶化,磁体的烧结温度范围较宽。磁体在烧结过程中高Dy含量合金主相晶粒中的Dy元素扩散到不含Dy元素的合金主相晶粒中,造成最后所得磁体中存在不同Dy含量的主相晶粒;磁体不同主相晶粒中Dy含量差别较大,随着添加Dy含量的增加,磁体中不同主相晶粒平均含Dy量也逐渐增加。     

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。     

添加Al、Mg、W、Mo对烧结Nd-Fe-B磁体磁性能与显微组织的影响

研究了在烧结ＮｄＦｅＢ磁体晶间添加Ａｌ、Ｍｇ、Ｗ、Ｍｏ等合金元素对显微组织和磁性能的影响。实验结果表明：低熔点合金元素Ａｌ、Ｍｇ能显著提高ＮｄＦｅＢ磁体的矫顽力，略微降低剩磁，对磁体的热稳定性无影响；高熔点合金元素Ｗ、Ｍｏ在不降低剩磁的情况下亦能提高磁体的矫顽力，但效果不如Ａｌ、Ｍｇ明显。显微组织分析表明，在添加低熔点和高熔点合金元素的磁体晶间发现了两种不同的新相。矫顽力的提高可归于晶间新相的出现。进一步分析表明，与传统的合金化相比，对ＮｄＦｅＢ磁体晶间区域进行微合金化是改进ＮｄＦｅＢ磁体组织与性能的一种更为有效的手段。     

烧结Nd-Fe-B磁体多主相复合制备及微观结构研究

利用双合金混粉法添加Dy实现烧结Nd-Fe-B磁体多主相复合制备,研究磁体的磁性能和微观结构。研究结果表明:单主相合金制备烧结Nd-Fe-B磁体时,主相晶粒中Dy含量差别不大,颗粒状富Nd相中所含Dy含量明显高于主相晶粒中所含Dy含量。双合金混粉法制备烧结Nd-Fe-B磁体时,能够提高磁体的取向,磁体中存在多主相晶粒复合;富Nd相中含Dy元素的总量降低,主相晶粒中含Dy元素的总量增加。烧结Nd-Fe-B磁体的多主相复合制备可以利用双合金混粉法得以实现;同时,相同合金成分时,双合金混粉法制备出的烧结Nd-Fe-B磁体的磁性能优于单合金法制备出的磁体,烧结Nd-Fe-B磁体的多相复合制备能够提高磁体的磁性能。     

Nd-(Fe,Co,Zr)-B纳米复合磁体的研究

利用XRD,TEM和DTA研究了不同淬火辊速度、晶化处理温度与时间对α-Fe／Nd2Fe14B型Nd10.5Fe78.8-xCo5.0ZrxB5.7纳米晶复合磁体结构和磁性能的影响规律。冷却辊速为25m·s^-1的Nd10.5Fe78.8-xCo5.0ZrxB5.7快淬态条屑具有纳米晶复合磁体结构,不经晶化处理就可获得较好的永磁性能。研究了Zr的添加和晶粒尺寸对性能的影响规律。添加0．5％（原子分数）Zr的合金进行700℃×10min的晶化处理后可获得较好的永磁性能。分析了微观结构和性能变化的机制。     

Nd-Fe-B磁体烧结过程晶粒长大行为的研究

定量描述了Nd-Fe-B磁体烧结过程晶粒长大行为，分析了烧结温度、烧结时间、合金粉末粒度及其分布对烧结过程晶粒长大的影响，讨论了烧结过程晶粒长大机制。在Nd-Fe-B磁体烧结过程开始之后的0—1h时间区段，晶粒长大迅速；随着烧结时间的延长，晶粒长大速度减小。合金粉末平均粒度增大，或者合金粉末粒度分布范围增宽，显著促进Nd-Fe-B磁体烧结过程中晶粒的长大。在Nd-Fe-B磁体的烧结过程中，存在两类晶粒长大机制，即Nd2Fe14B颗粒的溶解与析出、Nd2Fe14B颗粒的并合与长大。Nd2Fe14B颗粒的并合与长大不仅使磁体的平均晶粒尺寸增大，也使晶粒尺寸分布范围增宽，是烧结Nd-Fe-B磁体显微组织中出现异常大晶粒的根本原因。     

辅合金的粉末尺寸对烧结钕铁硼磁性能和微结构的影响

双合金法是降低烧结钕铁硼稀土特别是重稀土含量、改善磁体微结构的一种有效方法,其中辅合金的成分及形态起着至关重要的作用。采用粉末冶金的方法,借助SEM和直流磁特性测量系统对辅合金和磁体的微观结构及磁性能进行了分析。结果表明:辅合金粉末尺寸较大时,往往存在大量的中间相能直接进入磁体中形成较大的软磁特性的过渡相,从而损害磁体的磁性能。相反,辅合金粉末尺寸越小,中间相在烧结过程中元素不需要长距离的扩散而达到稳定状态,有利于优化微结构,提高磁体的磁性能。     

添加MgF2对烧结NdFeB磁体的性能和微观组织的影响

采用晶界添加MgF2制备烧结NdFeB磁体,通过扫描电镜、透射电镜和性能测试,研究了烧结NdFeB磁体的微观组织及其对磁性能、电阻率的提高和耐腐蚀性能的影响.结果表明:添加适量MgF2可实现在磁体剩磁、矫顽力和电阻率提高的基础上,同时提高材料的腐蚀电位,并且在极化曲线的阳极部分相同电位条件下,具有较小的极化电流密度,从而达到改善NdFeB磁体耐腐蚀性能的目的.磁体显微组织研究表明F元素进入晶界相,形成F含量约为30％(原子分数)、以面心立方为基的有序的NdOxFy相,其与磁性能、电阻率的提高和耐腐蚀性能改善有关.     

改进片铸与烧结技术制备高性能钕铁硼磁体的研究

通过优化合金成分设计与改进速凝片铸技术、烧结技术,应用国内通用的工业生产烧结钕铁硼磁体的各类原材料,在工业生产线上实现了45UH高性能烧结钕铁硼磁体的批量生产。SEM观察和XRD分析结果表明:磁体具有比较高的取向度;其显微组织致密、精细而均匀,平均晶粒尺寸约为5μm。45UH烧结钕铁硼磁体的典型磁性能为Br=1.363 T,Hcb=1060 kA.m-1,Hcj=2140 kA.m-1,Hk=1625 kA.m-1,(BH)max=366.0 kJ.m-3;其Hcj/79.6 kA.m-1+(BH)max/7.96 kJ.m-3=72.8。在295～453 K温度区间,其剩磁与内禀矫顽力的温度系数分别为-0.108%.K-1和-0.486%.K-1。当L/D=0.7时,在473 K保持2 h磁体开路磁通不可逆损失为4.1%左右。批量生产的45UH烧结钕铁硼磁体,其常温磁性能优异,温度稳定性良好。     

还原扩散法制备钐铁氮磁性材料的组织结构与性能研究

研究了还原扩散法制备Sm2Fe17Nx(x≈3)磁性材料的组织结构与性能。用DTA方法测定了Sm2Fe17Nx的热稳定性,用VSM测定了本实验所制Sm2Fe17Nx磁体的磁滞回线和退磁曲线;用TEM及高分辨电镜分析了渗氮前后Sm2Fe17合金及Sm2Fe17Nx结构。结果表明:Sm2Fe17Nx的分解温度为841 K,用还原扩散法制备的Sm2Fe17Nx磁粉做成粘结磁体后各向异性不是很强烈,性能偏低。Sm2Fe17Nx磁粉磁性的好差与渗氮层的厚度有密切的关系,渗氮后的Sm2Fe17Nx确实有体积膨胀的现象,而且属非晶结构。     

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.     

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。     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。