水菱钇型碳酸钕的形成及聚甘油脂肪酸酯对结晶的影响

Amorphous Neodymium carbonate was prepared by the precipitation reaction of neodymium chloride with ammonium bicarbonate in solution, and then aged at 60 ℃ to form crystalline neodymium carbonate. The feed molar ratio of n_(NH4HCO3)/n_(NdCl3 was 2.5, and the precipitation was carried out with or without addition of polyglyceryl fatty acid ester (PGFAE). The phase type and morphology of crystalline neodymium carbonates were examined by XRD and SEM, and the effect of PGFAE on the crystallization speed was investigated by volume change in deposit layer and in situ pH determination. The content of neodymium and chloride in crystals was analyzed, and the crystallization reaction or crystal growth characteristics were discussed. It was found that all the crystalline neodymium carbonates were tengerite type, and contained less crystalline water and chloride than that of lanthanite type neodymium carbonate crystallized at room temperature, which is beneficial to the production of neodymium carbonate with higher neodymium and lower chloride content. The addition of PGFAE not only could eliminate the foam formed during precipitation, but also could shorten crystallization time, and form large radiative-like shape conglomeration by the irregulative linkage of one dimension needle crystals. It is also suggested that the morphology and the chloride content of neodymium carbonate were dependent on the structure and crystal growth characteristics.     

碳酸氢铵与氯化钇反应及结晶产物的组成和晶相类型

The relationships of crystal type, crystallization speed, purity, grain size and shape of rare earth carbonate with precipitation and crystallization conditions are very important for the production of rare earth carbonate with high efficiency, high quality and low cost. It is necessary for us for further understand the crystallization process mechanism and the factors effect on the crystallization. In the present paper, the crystallization characteristic, composition and crystal phase type of yttrium carbonates or ammonium yttrium carbonates precipitated from yttrium chloride solution using ammonium bicarbonate as precipitant were determined by chemical analysis, X-ray powder diffraction and the pH situ-determination. It was found that the crystal phase type was dominated by the feed molar ratio of ammonium bicarbonate to yttrium chloride, and the crystallization speed and the crystal composition were also influenced by temperature, feed manner and aging period etc. When precipitating and aging under lower temperature, crystallization is easy to take place in the high feed molar ratio zone, and when increasing tempera-ture, crystallization will take place both in lower and higher feed molar ratio zones. The results show that spherical yttrium carbonate with tengerite type crystal phase can be formed within the temperature 30～70℃ when feed molar ratio of ammonium bicarbonate to yttrium chloride is less than 4, and that a rhombus flake crystal, which possesses the composition of ammonium yttrium quasi-double carbonate and a new XRD pattern, is formed when the feed molar ratio is over 4. Their compositions can be represented as (NH₄)_aY(CO₃)_b(OH)_c·nH₂O, a< 1, 1< b< 2, c=3+a-2b. A fine crystal of ammonium yttrium double carbonate with the formula of (NH₄)Y(CO₃)₂·H₂O can also be obtained as using an enough amount of ammonium bicarbonate and aging enough time.     

计算机模拟阴离子对碳酸镍结晶过程的影响

本文采用原子模拟技术,研究了不同溶液中碳酸镍的结晶行为。结果表明,水化作用使碳酸镍晶体更稳定,形貌更规整。杂质阴离子SO₄^2-与碳酸镍晶体表面的作用力较强,但对其形貌影响不大。Cl^-对表面的作用力较弱,但使晶体形貌更不规则。在模拟的几种情况中,碳酸镍的(104)晶面均是最主要的显露面。模拟结果能与实验现象很好吻合。     

超细碳酸钇热分解行为及焙烧工艺的研究

超细Y2O3同时具有尺寸效应和稀土元素的双重特性,有着更加特殊的性质,在陶瓷、发光材料等方面多有应用.目前工业上主要通过液相沉淀法获得超细前驱体,进而焙烧获得超细Y2O3;然而,在前驱体焙烧过程中,一般都需添加表面活性剂来避免团聚的发生,使焙烧前后产物的粒径和形貌具有良好的一致,最终获得粒度均匀的超细Y2O3;但表面活...     

碳酸镨的结晶活性、外观形貌及结晶生长机制

采用原位pH值测定法确定了碳酸镨的结晶活性区域,并用扫描电镜观测了不同结晶区域结晶碳酸镨的外观形貌.结果表明在低配比区域(NH4HCO3/PrCl3的摩尔比小于3)为碳酸镨的易结晶区域,结晶产物为交叉层叠的花瓣形颗粒;在高配比区域(NH4HCO3/PrCl3的摩尔比大于3)为碳酸镨的可结晶区域,延长陈化时间可以得到鱼鳞片状的亮晶产物;所有结晶碳酸镨都具有镧石型结构,其基本构筑单元为片状结晶,这与镧石的层状结构相关.影响结晶的主要因素是加料比,其它因素象温度,加料方式和搅拌强度等对结晶过程也有影响.     

二氧化碳碳化沉淀制备碳酸钇的反应过程研究

CO₂碳化沉淀制备特殊物性金属化合物粉体具有成本低、操作简单等优点,已成功应用于纳米、大比表面稀土氧化物的制备。以Y元素为研究对象,针对酸/碱体系下CO₂碳化沉淀制备碳酸钇的反应过程进行研究。结果表明,氯化钇的引入会迅速与H₂CO₃-H₂O体系中的HCO₃^-离子反应生成Y₂(CO₃)₃·xH₂O,从而促进H₂CO₃的电离,导致pH小于9.0的溶液中HCO₃^-的占比小于1%。在酸性体系下,CO₂首先发生溶解吸收电离,然后Y³⁺与HCO₃^-反应进行沉淀,而NaOH的加入中和了反应释放出的H⁺,从而控制碳化体系pH;整个碳化过程符合一级反应动力学模型,由传质扩...     

铈硝酸盐及其硝酸铵复盐的结晶制法及性质

通过对硝酸铈、硝酸铈铵复盐的制备,叙述了硝酸铈的溶解度[1]、复盐形成等性质, 分析了结晶方式不同对铈硝酸盐及其硝酸铵复盐产品质量的差别, 指出通过改变其传统的结晶法制备工艺, 提高产品质量具有重要的现实意义.     

镧石型碳酸钕的形成及晶种对结晶的促进作用

The characteristics of pH value variation during aging process of amorphous neodymium carbonate formed by three different feeding manners have been investigated. The promotion action of seeding on the crystallization of neodymium carbonate is discussed. X-ray diffraction pattern and the elemental analysis results show that neodymium carbonate can transfer from amorphous to crystalline normal neodymium carbonate Nd₂(CO₃)₃·8H₂O with lanthanide structure at room temperature. Its crystallization activity zone lies in lower feeding ratio area expressed by n_NH4HCO3/n_NdCl3 between 2～3. The existing of seeds can shorten crystalline time, from more than 15 h without seed to 2 h with seeds under normal feeding manner. And the spontaneity nucleation time can be shortened further when feeding with multi-steps normal manner. However, whether multi-steps normal or synchronously and continuously feeding manner, the precipitate formed can transfer to crystalline neodymium carbonate directly under seeding. At the same time, it is observed that the variation of pH value reduces with the decrease of feeding amount and the shortening of aging period, indicating that with synchronously and continuously feeding manner can not only realize fast crystallization, but also control pH value within a narrow range, which is beneficial for the producing of neodymium carbonate crystal with narrow-distributed particle size and monitoring of its crystallization process.     

结晶碳酸钕的水热合成、外观形貌及其组成

Crystalline neodymium carbonates were prepared by treating the amorphous precipitate formed from the reaction between neodymium chloride and ammonium bicarbonate under hydrothermal condition. Their composition, morphology and crystal phase were identified by means of elemental analysis, SEM and XRD. It was found that Nd₂(CO₃)₃·2.5H₂O with tengerite-type structure and sheet morphology was obtained when the feed molar ratio(FMR=n_(NH4)2CO2/n_NdCl3)was 2 or 1.8 and hydrothermally treated at 150 ℃ for 12h. However, orthogonal NdOHCO₃ particles agglomerated with long rod crystals were formed when lowering FMR to 1.5 under the same hydrothermal condition. Phase transformation from tengerite-type Nd₂(CO₃)₃·2.5H₂O to orthogonal NdOHCO₃ was occurred when increasing hydrothermal temperature or prolonging hydrothermal time, which is beneficial to the preparation of neodymium hydroxyl-carbonate with neodymium oxide content higher than 70%.     

含钇WC—Co系硬质合金中钇相的电子显微镜研究

近年的研究表明,在WC-Co系硬质合金中加入微量稀土元素,能提高合金的抗弯强度、韧性、耐磨性和抗冲击性,并可成倍地提高合金刀具的使用寿命。但有关机理的研究还只是开始,尤其是对稀土元素在合金中的存在方式和分布状态还缺乏较为深入的研究。本文采用电子显微术、能谱和能量损失谱分析等方法研究了含钇的WC-Co系硬质合金中钇相的相结构、相成分及周围的显微组织,并对钇在合金中的分布状态以及钇对合金性能的几种可能的作用机理进行了探讨。     

稀土离子对溶液体系中碳酸钙生成的影响

用X射线粉末衍射、XPS光电子能谱、红外光谱以及ICP-MS等技术研究不同浓度的Ce3+,Nd3+,Tb3+,Gd3+,Lu3+对碳酸钙结晶状况的影响.稀土离子的加入有利于热力学稳定态的方解石型碳酸钙的生成,并且稀土离子能够部分的取代晶格中的钙离子,改变碳酸钙的结晶习性,在宏观上形成有序规则的排列.     

碳铵沉淀法制备纳米氧化钇过程中氯离子的行为

研究了碳酸氢铵沉淀法制备纳米氧化钇过程中氯离子的行为及去除方法,认为沉淀物的组成为Y(OH)0.1Cl0.1(CO3)1.4·2H2O。讨论了氯离子的存在形式,氯离子主要以氯化铵吸附或夹带和碳酸钇复合物的形式存在,其中碳酸钇复合物和颗粒内部夹带的氯离子是影响最终纳米氧化钇中氯含量的关键。通过实验研究证明采用洗涤和提高煅烧温度和延长保温时间可以有效减少氯离子的含量,制得了氯离子含量为0.054%的纳米氧化钇粉体。     

The Aggregation Kinetics of Colloidal Particles of Basic Yttrium Carbonate

Studyofthegrowthprocessofcolloidalparticlesofnonequilibriumandirreversibilityisanactiveareaofresearch.Therecognitionofcolloidalaggregatesasfractalobjectshasinspiredalargenumberofexperimentalandtheoreticalstudiesonthestructuralandkineticaspectsofaggregationprocesses"'.Morerecently,kineticsofhematiteaggregationbypolyacrylicacidhavebeenstudiedbyzhangandBume3.Theprimaryhematiteparticleswerequiteuniformandfairlyspherical.Inthispaper,wewillreportthesizeevolutionoffractalaggregatesofinitiallypolydis…     

钇对Fe-Cr-Al合金循环氧化行为的影响

用热重分析、扫描电镜及能谱分析等手段研究了合金中弥散分布的Ｙ、弥散分布的Ｙ２Ｏ３及离子注入Ｙ＾＋对Ｆｅ－２３Ｃｒ－５Ａｌ合金１１００℃循环氧化行为的影响,不含Ｙ的合金比１００ｈ循环氧化后氧化膜发生了开裂和剥落,露出合金基体;加入弥散的Ｙ或Ｙ２Ｏ３的合金经１００ｈ循环化后氧化膜平坦致密,不剥落,离子注入１＊１０＾１７Ｙ＾＋／ｃｍ＾２后合金氧化膜主要发生层间剥落。Ｙ提高Ｆｅ－Ｃｒ－Ａｌ合金氧化膜粘附性     

钇对Fe-Cr-Al合金氧化膜粘附性的影响

利用热重分析,扫描电镜及能谱分析等手段研究了合金中弥散分布的Ｙ,Ｙ２Ｏ３及离子注入Ｙ＾＋对Ｆｅ－２３Ｃｒ－５Ａｌ合金１１００℃恒温氧化行为的影响。不含Ｙ的Ｆｅ２３Ｃｒ５Ａｌ合金氧化膜起皱,长时间氧化后冷却过程中膜发生开裂剥落。合金离子注入１＊１０＾１７Ｙ＾＋／ｃｍ＾２后氧化膜粘附性得到了改善。合金中加入弥散的Ｙ或Ｙ２Ｏ３改变了氧化膜形貌,膜平坦致密,不开裂剥落,不含Ｙ的Ｆｅ２３Ｃｒ５Ａｌ合金氧化膜皱褶形貌的形成及膜发生剥落的原因与氧化膜生长机制及合金中Ｓ的界面偏聚有关,Ｙ提高Ｆｅ－Ｃｒ－Ａｌ合金氧化膜粘附性的原因主要在Ｙ易与Ｓ形成稳定的硫化物,从而阻止了Ｓ在膜／合金界面偏聚。Ｙ提高Ａｌ２Ｏ３膜粘附性的原因还在于改变了Ａｌ２Ｏ３膜的生长机制。     

添加钇提高不锈钢耐蚀性能的AES研究

用俄歇能谱仪对比研究了添加０．２％Ｙ对高硅不锈钢在９３％Ｈ２ＳＯ４介质中所形成的钝化膜中各元素浓度分布的影响，添加０．２％Ｙ增大了ＳｉＯ２在不锈钢钝化膜中的比例，从而使合金中Ｓｉ可充分形成富ＳｉＯ２的钝化膜。     

钇对2618合金组织及性能的影响

采用X射线，光学显微镜及扫描电镜等手段研究了2618合金中的组织与相结构，并研究了元素钆在2618合金中的存在形式及其对合金力学性能的影响。结果表明，微量钆元素在铝合金中是以化合物形式存在的；钆对合金中的铸态组织及Al9FeNi仃形态没有影响。由于微量钆的加入，降低了铜与镁在2618合金中的固溶量，减少了时效析出相A2CuMg数量，从而降低2618合金的室温强度帮在250℃的高温瞬时强度；但由于微量钆减少了铜与镁在2618合金中的扩散速度，延缓了时效机的粗化，并由于第二相数量的增多，因此提高了2618合金在250℃经100h高温热暴露后的高温瞬时强度。     

磷酸铵镁法回收稀土分离废水中镁及氨氮的研究

磷酸铵镁法是一种有效的回收氨氮、磷和镁的方法。本文通过热力学计算,分析了反应过程及pH值对磷酸铵镁生成的影响规律。根据理论分析结果,进行了pH值、磷源、加料方式等因素对氨氮、磷去除率的影响实验。结果表明:以Na3PO4为磷源,通过向氮磷混合液中加入含镁废水,并控制反应液pH值为9时,氮磷镁去除率均可达98%以上,得到沉淀物经X衍射分析为六水磷酸铵镁。