Mg-Zn-Zr-RE系镁合金中的稀土相分析

用光学显微镜、电子探针、X射线衍射及电手显微分析等手段研究了Mg Zn Zr RE合金铸态及挤压态的稀土相。在铸态组织中,稀土及锌均富集于晶界,形成三元金属间化合物Mg_3RE_2Zn_3(W)相及Mg_3REZn_6(Z)相,在0.8Y和0.79RE合金中以Z相为主,而在2.56RE合金中W相多于z相;挤压型材中均存在W和Z相。铸态合金经350℃保温并挤压后,合金发生如下相变:Mg+Mg_3REZn_6(Z)→MgZn+Mg_3RE_2Zn_3(W)实验测定了Z相为六方结构,其a=0.640～0.642nm,C=1.029～1.031nm。     

富钇混合稀土和热处理对Mg—Zn—Zr系镁合金的组织及相结构的影响

富钇混合稀土对Mg-Zn-Zr系镁合金的铸造组织及组成相无显著影响。MB25合金(含高纯金属钇)和MB26合金(含富钇混合稀土)的铸造组织都是在α-Mg晶界上分布着大量的Z+β网状共晶化合物相(以Z相为主),其区别在于铸态MB26合金的晶界共晶相中溶有少量的镧、铈、错、钕、钆和镝等多种稀土元素。均匀化处理和挤压热加工都能使铸态MB26合金发生不同程度的相变,并在不同程度上改变铸态合金的组织和相结构。随着从挤压到均匀化处理温度的提高,其相变过程是从Z相中锌的扩散相变开始到β、W共晶相各自完成共析转变结束。     

钇对Mg-0.8Zr-0.35Zn基合金组织及高温性能的影响

采用XJG-04型金相显微镜、 JCXA-733电子探针、 D/max-rB型X射线衍射仪及WDW-200型电子万能实验机研究了Y对Mg-0.8Zr-0.35Zn基合金铸态、固溶时效组织及高温(250 ℃)性能的影响. 结果表明: Y能细化Mg-0.8Zr-0.35Zn基合金铸态及热处理态组织, 加入Y形成新相Mg24Y5. 在250 ℃时, 随着Y含量增加合金高温抗拉强度增大, 延伸率及断面收缩率降低; 高温拉伸断口SEM图像显示脆性断裂趋势增大, 断裂由延性向解理方式发展.     

Mg—Zn—Zr—Y系镁合金的X射线衍射分析

采用X射线衍射方法,对铸态Mg-Zn-Zr-Y系列合金基体相(α-Mg)的面间距(d值)变化及析出相进行了研究。结果表明,α-Mg的d值随着钇含量的增加先增大,随后变小。在不含钇的合金中,析出相主要是MgZn及MgZn_2;在含钇合金中,钇小于0.94 wt％时,晶界相主要是Z相;钇含量高于0.94 wt％后,逐渐转变为以W相为主。除了上述相外,在含钇合金中还出现Y-Zn及Mg-Y相。     

往复挤压准晶增强快速凝固Mg92.5Zn6.4Y1.1合金

采用往复挤压工艺将快速凝固Mg92.5Zn6.4Y1.1合金薄带在330℃挤压2道次和4道次,然后正挤压制成Φ10 mm的棒材。用OM,TEM,XRD及DTA研究了往复挤压过程中准晶相I-Mg3YZn6弥散析出及对力学性能的影响。研究表明,往复挤压有利于快速凝固Mg92.5Zn6.4Y1.1合金薄带的焊合,获得组织致密、均匀、高强韧合金。往复挤压2道次,相组成为-αMg和准晶I-Mg3YZn6,脱溶析出纳米准晶相较少;4道次相组成为-αMg和准晶I-Mg3YZn6及MgZn相,脱溶弥散析出的纳米I-Mg3YZn6准晶相及MgZn相较多。往复挤压提高材料的拉伸性能,其主要原因是细晶强化和析出强化。     

锌对稀土镁合金组织与力学性能的影响

采用OM, XRD, SEM和EDS等试验手段研究了Zn对稀土镁合金Mg-4Y-1Ca(%,质量分数)微观组织和力学性能的影响。结果表明:随着Zn (x=1%, 3%, 5%)的加入, Mg-4Y-1Ca合金中生成的Mg_(24)Y_5二元相逐步转变为Mg_3Y_2Zn_3(W相)+Mg_(12)YZn(X相)三元相,铸态组织细化,第二相沿晶界成网状分布;经热挤压变形后,合金再结晶后晶粒细化明显,第二相弥散分布于基体和晶界上,强度提高的同时伸长率也获得较大提升,其中Mg-4Y-1Ca-5Zn合金表现最为显著。得益于Zn添加对再结晶晶粒细化和W相、 X相弥散强化的共同作用, Mg-4Y-1Ca-5Zn合金经热挤压处理后具有较佳的综合力学性能,屈服强度、抗拉强度和伸长率分别达到198 MPa, 271 MPa和24.6%。     

锌含量对铸态Mg-10Y-xZn-0.5Zr镁合金微观组织和力学性能的影响EI北大核心CSCD

采用光学显微镜、扫描电镜、X射线衍射仪、透射电镜、电子拉伸实验机等研究了铸态Mg-10Y-xZn-0.5Zr(x=1,1.5,2(%,质量分数))合金的微观组织和力学性能。结果表明:铸态Mg-Y-Zn-Zr合金组织主要由α-Mg,LPSO相和W相组成,其中LPSO相的化学式为Mg_(12)YZn,W相的化学式为Mg_(3)Zn_(3)Y_(2)。LPSO相主要呈块状或层片状,随着Zn含量的增加,块状LPSO相体积分数逐渐增多,同时合金的屈服强度逐渐增加。当Zn含量为2%时,LPSO相形貌表现出以块状相为主,铸态Mg-10Y-2Zn-0.5Zr合金具有最佳的综合力学性能,其屈服强度、抗拉强度和延伸率分别为123.9,206.2 MPa和12.06%。块状LPSO相体积分数的增加是合金力学性能提高的主要原因。     

退火温度对La0.75Mg0.25Ni3.5Co0.2贮氢电极合金的结构及电化学性能的影响

为了改善La-Mg-Ni系合金电极的循环稳定性,对铸态合金La0.75Mg0.25Ni3.5Co0.2在0.3 MPa压力氩气保护下进行不同温度的退火（1123,1223和1323 K）,保温时间均为10 h。系统研究了退火温度对合金的微观结构及电化学性能的影响。X射线衍射（XRD）和扫描电镜（SEM）研究结果表明,合金具有多相结构,当铸态及1123 K温度退火后合金主要由LaNi5,（La,Mg）2（Ni,Co）7相以及少量的LaNi2相组成。当退火温度为1223和1323 K时,合金中LaNi2相消失,合金主要由LaNi5,（La,Mg）2（Ni,Co）7及（La,Mg）（Ni,Co）3相组成。随退火温度提高,合金最大放电容量单调下降,但合金的循环稳定性得到改善。退火处理改善合金循环稳定性的原因在于退火后合金组织均匀,晶粒增大,在KOH电解质溶液中增强合金电极抗氧化腐蚀能力,抑制合金颗粒粉化。     

钇对Mg-5Zn-2Al合金组织和力学性能的影响

利用金相显微镜、电子万能试验机、扫描电镜和X射线等手段,研究了不同含量的Y对Mg-5Zn-2Al镁合金铸态及热处理状态下组织及力学性能的影响.结果表明:合金主要由α-Mg基体相、Mg32(Al,Zn)49相及Al3Y相组成,并且A13Y稀土相随着合金中加Y量的增加而增多.在铸态及热处理条件下,合金的力学性能(抗拉强度和延伸率)均呈现先下降后上升的变化趋势.在铸态条件下,当加Y量为0.3%时合金的抗拉强度达到最大,为205 MPao当加Y量为0.9%时,合金的延伸率达到最大,为14.6%.经过T6热处理后,合金的抗拉强度较铸态均得到了明显提高,而延伸率有所下降.加Y量为0.9%的Mg-5Zn-2Al镁合金的抗拉强度和延伸率均达到最大值,分别为234 MPa和11.4%.     

铸态Mg-Sm-Gd-Zn-Zr合金微观组织与力学性能研究

采用光学显微镜、X射线衍射仪、扫描电子显微镜、透射电子显微镜、拉伸试验机研究了铸态Mg-xSm-yGd-Zn-Zr(x = 3,y =5;x = 4,y=4;x = 5,y=3(％,质量分数))合金的微观组织和力学性能.铸态合金中存在面心立方结构的(Mg,Zn)3(Sm,Gd)相,a = 0.726 nm.三种铸态合金...     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.