制取氮化锰工艺和技术

介绍了利用金属锰粉采用固态氮化法生产氮化锰的原理和工艺。采用正交设计法,在实验室管式炉内、高温条件下利用氨气分解产生的活性氮对锰粉进行氮化获得氮化锰粉,通过一系列实验得出了适宜的技术工艺参数;锰粉粒度、氮化温度和氮化时间。获得了含氮高达6．880％－6．902％的氮化锰产品.     

金属锰氮化的动力学研究

应用真空电阻炉高温渗氮、X射线衍射、惰气熔融法氧氮分析等实验测试方法,研究了金属锰在1173K含氮气氛中的氮化及动力学规律。渗氮时间愈长,试样的氮化量愈多。除有微量的MnO生成外,随渗氮时间的延长,金属锰可全部氮化为Mn4N和ζ-(Mn2N)。建立了金属锰氮化的动力学模型,与实验结果基本符合,能较好地反映氮化规律。     

金属锰渗氮及热力学分析

应用真空电阻炉高温渗氮、X射线衍射、惰气熔融法氧氮分析等实验测试方法 ,研究了粒度、渗氮时间等因素对金属锰渗氮的影响。粒度愈小 ,渗氮速度愈快。随渗氮时间的延长 ,除发生微量氧化生成MnO外 ,金属锰可全部氮化为Mn4 N和少量Mn2 N .应用规则溶液模型和有关研究报道计算得到 ζ相 (计量组成为Mn4 N )的生成自由能 :ΔG0 Mn4 N =- 110 85 0 (±30 0 0 ) + 6 4.714 (± 2 .2 )T(J/mol) .     

金属锰JMn93A渗氮的实验研究

应用真空电阻炉高温渗氮,X射线衍射分析等实验测试方法,研究了粒度,温度,气相组成等因素对金属锰渗氮的影响,工业用气态氮作为渗氮气体的主要气相组成,可同时发生金属锰的氮化和氧化,生成Mn4N和MnO化合物,随渗氮温度的提高,锰氧化物的含量相应增高,渗氮气氛中配加氨气,使氨气的分压相应降低,平衡吸附浓度降低。渗氮试样的含氮量降低。     

添加合金元素Cu和Mn对锆合金中第二相的影响

以Zr-4为母合金,分别添加电解纯铜或电解金属锰,用非自耗真空电弧炉熔炼了成分不同的6种锆合金.用透射电子显微镜观察了合金中第二相的形貌,用EDS分析了第二相的成分,用SAD确定了第二相的晶体结构.添加Cu元素的合金中有3种第二相：Zr(Fe,Cr)₂粒子、Zr(Fe,Cr,Cu)₂粒子和含少量Fe或不含Fe的Zr-2Cu粒子;添加Mn元素的合金中只有1种Zr(Fe,Cr,Mn)₂第二相,且随着合金中Mn的质量分数从0.07%增加到0.35％,Zr(Fe,Cr,Mn)₂粒子中Mn元素的质量分数也升高.     

大型水轮机叶片马氏体不锈钢的超声空蚀行为

利用超声振荡空蚀设备研究了一种大型水轮机马氏体不锈钢合金成分调整前后在蒸馏水和模拟长江水中的空蚀行为.观察空蚀表面形貌,结合力学性能,与普通13-4不锈钢进行对比分析.研究结果表明:3种不锈钢的显微组织由马氏体、铁素体和残余奥氏体组成;降低C,S,Si增加Ni,Mo,Mn并且经过精炼工艺改进后,不锈钢抗空蚀能力高于原合金和13-4不锈钢.调整后不锈钢的空蚀稳定期失重率小于7 mg/h,仅约为原合金的75%和13-4不锈钢的25%.在空蚀过程中,较软的铁素体相首先脱落,其次是较硬的马氏体相,并且观察到了清晰的空蚀表面疲劳源形貌.     

自蔓延法制取锰铝中间合金的实验

首次将自蔓延高温合成法（self-propagating high-temperature synthesis,SHS）用于锰铝中间合金的制备。采用Miedema生成热模型、金属间化合物的双参数模型估算了锰铝中间合金的标准生成焓、标准熵及比热容。通过理论计算确定了Mn3O4-Mn2O3-CaO-Al反应体系的绝热温度。以Mn2O3、Mn3O4和CaO、金属Al为原料,进行了锰铝中间合金的自蔓延反应合成试验,采用化学滴定、X射线衍射以及光学显微镜的方法对产物进行分析。理论计算和实验结果表明：反应体系的绝热温度为3 160 K,确定了该体系进行自蔓延反应的可行性。采用自蔓延合成法制备出了锰含量高达78%以上的锰铝中间合金,拓宽了锰铝中间合金的生产工艺。     

利用离子膜电解槽在氯盐电解质中电沉积金属锰

对阴离子交换膜电解槽在氯盐电解质中电沉积锰进行研究,并采用循环伏安法对其进行电化学分析。研究结果表明:电解最佳条件是锰离子浓度为0.9 mol/L,氯化铵浓度为2.4 mol/L,电解温度为40℃,电流密度为450A/m2,pH为7.3,SeO2浓度为0.36 mmol/L,在此条件下,金属锰的电沉积效率为90.8%,电耗为4 816 kW·h/t;其晶型为γ型;利用离子膜电解槽电沉积金属锰能有效地防止阴极表面Mn2+的浓差极化,提高电流效率,该过程所发生的还原反应为扩散过程控制。     

CuMn35中间合金的研制

介绍了用熔融法生产CuMn35中间合金的原理和方法,并讨论了熔炼过程中脱氧和除氢等问题.通过正交实验,得出熔炼CuMn35中间合金的最佳工艺条件为:冶炼温度为1 200 ℃,冶炼时间20 min,熔剂占总炉料的最佳百分比为2.0%.采用快速熔化和急冷技术获得成分均匀的产品.采用木炭和Na3AlF 6作为覆盖剂和精炼剂处理可以提高产品的表面质量,减少杂质含量,提高Cu、Mn的收得率(分别达到99.99%和99.31%).实验结果表明,采用的工艺和方法是可行的.     

Mn3+/Mn2+间接电氧化法分解辉钼矿

采用Mn3 /Mn2 间接电氧化法湿法分解辉钼矿.在强酸介质中,媒介Mn3 /Mn2 氧化能力很强,能将MoS2氧化分解为MoO3和硫酸,且锰离子可以循环利用.探讨了Mn3 /Mn2 间接电氧化法的工艺条件,结果表明:在H2SO4浓度为7 mol/L,MnSO4浓度为0.5 mol/L,电解电量为20 A·h·g-1,电极间距15 mm,阳极电流密度为800 A·m-2,矿浆液固比为40,温度为55 ℃的条件下,钼的浸出率为88.5%.此外,对氧化浸出过程采用了超声波外场强化,Mo浸出率可以提高到92.3%.     

Nitridation of chromium powder in ammonia atmosphere

CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were constructed for different temperatures. Chromium nitride formed at 7002-1200℃ under relatively higher nitrogen and lower oxygen partial pressures. Phases in the products were then investigated using X-ray diffraction (XRD), and the Cr₂N content varied with reaction temperature and holding time. The results indicate that the Cr metal powder nitridation process can be explained by a diffusion model. Further, Cr₂N formed as an intermediate product because of an incomplete reaction, which was observed by high-resolution transmission electron microscopy (HRTEM). After nitriding at 1000℃ for 20 h, CrN powder with an average grain size of 63 nm was obtained, and the obtained sample was analyzed by using a scanning electron microscope (SEM).     

基于层状磷酸锰-金纳米颗粒复合物的电化学传感器研究

利用化学沉淀方法室温下水相合成层状磷酸锰纳米材料.然后利用磷酸锰-金纳米颗粒修饰玻碳电极,构建电化学传感器并用于多巴胺的灵敏检测.通过循环伏安法和微分脉冲伏安法对所构建传感器的电化学行为进行考察.结果表明,该传感器对多巴胺的线性检测范围为0.5~120μmol/L,检出限为0.05μmol/L.同时,该方法具有灵敏度高、抗干扰能力强、稳定性好等优点.     

铟氮共掺杂氧化锌在可见光下的光催化活性

铟氮共掺杂氧化锌采用两步法合成,首先采用共沉淀方法制备铟离子掺杂的氧化锌,然后采用氨气中退火的方法制备铟氮共掺杂氧化锌.研究表明共掺杂样品比只掺杂氮的样品具有更多的可见光吸收.采用可见光下对异丙醇的降解来评价样品的光催化活性.研究结果表明在氮离子和0.5%铟离子掺杂下具有最好的光催化活性.     

临界氮势控制及影响因素

应用氮势进行可控渗氮时,须用不同温度下出现化合物相的临界氮势曲线,作为可控渗氮工艺的主要依据。本文在建立临界氮势曲线计算方法及结果基础上,分析温度、时间、合金元素含量、渗氮气氛对临界氮势曲线的影响,得出结论:调整渗氮温度、渗氮气氛和氨流量,通过气氛氮势的变化,可有效地控制化合物层的形成。     

Investigation on preparing boron nitride by nitriding pure boron at 1200–1550 1C

Boron nitride (BN) was prepared by nitriding pure boron (B) deposited on carbon substrates by chemical vapor deposition (CVD). Thermodynamic analysis of preparing BN by nitriding CVD B at 1200–1550 1C was firstly performed. And then, the effects of nitridation conditions, including temperature, nitridation atmosphere and CVD B microstructure, on the conversion of B to BN were analyzed by scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Results show that the conversion degree of B to BN firstly increased and then slightly decreased with rising temperature. The nitridation degree was controlled by mutual actions between the nitridation of B and consumption of the effective nitrogen source (NH3). The morphology of products and the reaction mechanism between B and N were influenced by nitridation temperature. At high temperatures (1400–1500 1C), BN with highly ordered microstructure was produced. On using N2–H2 as nitridation atmosphere instead of NH3–H2– N2, no BN was obtained in the studied temperature range. The microstructure and component of BN obtained in nitridation process were little affected by the microstructure of CVD B.     

Microstructure evolution of Ti–6Al–4V under cold rolling + low temperature nitriding process

A new nitriding process modifying both the surface and the matrix is proposed to improve the poor wear resistance and low hardness of the titanium alloy surface. The treatment of solid solution treatment, cold rolling and low temperature nitriding was used for surface modification. The results showed that the microstructure of the Ti–6Al–4V(TC4) titanium alloy sample changed from the original α+β phase to the residual α phase, metastable β phase and martensite α′ phase after solution treatment. The results of cold rolling experiments indicated that with the increase of rolling amount, many defects generated, and the grains were first elongated and then partially broken. During the process of low-temperature nitriding the recrystallization occurred, which effectively avoided the problem of coarse matrix structure. It has been found that after low-temperature nitriding, thin strip-like α-phase with dispersed distribution, which is a typical aging structure, formed. The XRD test results indicate that steady state nitrides Ti₂N formed on the surface of the sample, but the content of Ti₂N was relatively low. Based on the morphology of content of the surface and cross-section it is believed that a special type of nitriding layerformed after low-temperature nitriding. The mechanical performance test results indicate that the wear resistance and hardness of the alloy increased significantly.     

Ag掺杂类钙钛矿Ca(Mn_2Cu_1)Mn_4O_(12)的电磁性能

采用固相反应法制备了系列Ca(Mn2Cu1)Mn4O12/mAg2O多晶类钙钛矿锰氧化物。X射线衍射表明,m≤0.3的样品呈比较纯净的类钙钛矿相,而m>0.3的样品,是由类钙钛矿和金属Ag相组成的复合物。所有样品呈现半导体导电性质,电阻率低于未掺杂的Ca(Mn2Cu1)Mn4O12样品。居里温度测量表明,随着Ag掺杂量的增加,样品的居里温度逐渐升高。对于m=0.3和m=0.6的样品,120K温度和1T磁场下磁电阻比可达-10%左右。