多组分硫酸体系P507萃取分离铈(Ⅳ)工艺

本文对２－乙基己基膦酸单２－乙基己基酯（Ｐ５０７）从含有Ｃａ２＋、Ｆｅ３＋、Ｆ－、ＰＯ３－４、Ｔｈ４＋、Ａｌ３＋、Ｍｎ２＋的多组分硫酸稀土溶液中一步萃取分离铈（Ⅳ）工艺进行研究,得到纯度≥９９．９％的氧化铈产品及少铈碳酸稀土产品（ＣｅＯ２／ＲＥＯ≤３％）。     

用稀土皂化有机相技术在轻稀土分离工艺中的新应用

采用Ｐ＿（２０４）萃取剂，氮化轻稀士为原料，应用稀土皂化有机相技术，连续、稳定地生产出９９～９９．５％的Ｎｄ＿２Ｏ＿３、镧铈谱富集物及部分９９～９９．５％Ｌａ＿２Ｏ＿３。且富集物ＬａＣｅＰｒ溶液稀土浓度提高了２～３倍，使下步工序的Ｃｅ－ｐｒ、Ｌａ－Ｃｅ分离段，在相同设备、萃取参数条件下，较原设计工艺提高处理量近５０％。     

高碱度控制氧位渣系（BaO—BaCl2—Cr2O3）对含铬铁水选择氧化脱磷影响的研究

在实验室条件下，以小渣量研究了ＢａＯ－ＢａＣｌ２（或ＢａＦ２）－Ｃｒ２Ｏ３系脱磷剂对高铬铁水脱磷时，脱磷剂中溶剂（ＢａＣｌ２和ＢａＦ２），氧化剂（Ｃｒ２Ｏ３和Ｆｅ２Ｏ３），渣量，铁液中原始〔％Ｃ〕和〔％Ｓｉ〕，以及温度对脱磷率的影响。     

高碱度控制氧位渣系（BaO－BaCl_2－Cr_2O_3）对含铬铁水选择氧化脱

在实验室条件下，以小渣量研究了ＢａＯ－ＢａＣｌ＿２（或ＢａＦ＿２）－Ｃｒ＿２Ｏ＿３系脱磷剂对高铬铁水脱磷时，脱磷剂中溶剂（ＢａＣｌ＿２和ＢａＦ＿２）。氧化剂（Ｃｒ＿２Ｏ＿３和Ｆｅ＿２Ｏ＿ｓ）、渣量、铁液中原始（％Ｃ）和（％Ｓｉ），以及温度对脱磷率的影响。     

纳米晶Fe_3B/Nd_2Fe_(14)B粘结永磁体的磁性能研究

本文研究了粘结剂含量和温度－时间变化对纳米晶Ｆｅ３Ｂ／Ｎｄ２Ｆｅ１４Ｂ粘结永磁材料的磁性能影响。结果表明降低粘结剂含量可显著地提高纳米晶Ｆｅ３Ｂ／Ｎｄ２Ｆｅ１４Ｂ粘结永磁的磁性能；环境温度对纳米晶Ｆｅ３Ｂ／Ｎｄ２Ｆｅ１４Ｂ粘结永磁的磁性能具有重要影响，在较高的温度下其磁性能将显著下降，因此纳米晶Ｆｅ３Ｂ／Ｎｄ２Ｆｅ１４Ｂ粘结永磁只能在较低的温度环境下使用     

水热法合成BaNd_xFe_（12－x）O_（19）铁氧体的研究

本文利用水热法合成了六角形磁铅石结构的ＢａＮｄｘＦｅ（１２－ｘ）Ｏ（１９）铁氧体，用Ｘ射线衍射仪、透射电子显微镜和振动样品磁强计等仪器对粉末的结构、形貌和磁学性能进行了研究，并讨论了Ｎｄ（３＋）对钡铁氧体磁学性能的影响。结果表明，Ｎｄ（３＋）可以明显提高ＢａＦｅ（１２）Ｏ（１９）粉末的矫顽力。     

氟碳铈矿热分解行为的研究

采用ＸＲＤ法分析了不同温度下氟碳铈矿焙烧分解产物的组成，探讨了氟碳铈矿的热分解过程。试验结果表明氟碳铈矿的热分解是分步进行的。首先（Ｃｅ，Ｌａ）ＣＯ３Ｆ分解成（Ｃｅ，Ｌａ）ＯＦ；升高焙烧温度，（Ｃｅ，Ｌａ）ＯＦ发生相分解，生成Ｃｅ０．７５Ｎｄ０．２５Ｏ１．８７５和（Ｃｅ，Ｐｒ）Ｌａ２Ｏ３Ｆ３两相；随着焙烧温度的继续升高，（Ｃｅ，Ｐｒ）Ｌａ２Ｏ３Ｆ３可分解为ＬａＦ３、Ｃｅ２Ｏ３、ＰｒＯ１．８３等相。焙烧过程中Ｃｅ３＋、Ｐｒ３＋氧化为四价，没有明显的脱氟行为。     

降低Nd_2O_3中杂质Sm_2O_3的工艺研究

在工业生产实践中，对Ｎｄ－Ｓｍ分组采用大捞大洗和加氨水强化萃取分离的工艺方法实现了一步萃取法除去Ｌａ３＋Ｃｅ３＋Ｐｒ３＋Ｎｄ３＋萃余液中Ｓｍ３＋的目的，经六个月运行，产品Ｎｄ２Ｏ３中杂质Ｓｍ２Ｏ３含量稳定在０．０３％以下。     

超微粉末NdFeO_3的制备及催化作用

本文采用溶胶－凝胶法合成了ＮｄＦｅＯ３超微粉末催化剂，Ｘ射线衍射结果表明产物单一，ＳＥＭ和ＢＥＴ法测得平均粒径小于０．１２μｍ，６００℃灼烧得与钙钛矿相关的ＧｄＦｅＯ３结构类型，属于正交晶系。催化实验表明ＮｄＦｅＯ３作为ＮＯ转化为Ｎ２的催化剂具有良好的催化性能     

用以磷酸三丁酯为载体的乳状液膜提取钕（Ⅲ）的研究

用磷酸三丁酯－Ｓｐａｎ８０－二甲苯乳状液膜体系研究了Ｎｄ（Ⅲ）的迁移行为。当膜相组成为０．０４０ｍｏｌ／Ｌ磷酸三丁脂和３％（ｗ／ｖ）Ｓｐａｎ８０，内相为０．１５ｍｏｌ／ＬＮａ２Ｓ２Ｏ３，外相为２．５ｍｏｌ／ＬＨＮＯ３，Ｎｄ（Ⅲ）能快速并完全迁移。常见过渡元素离子Ｆｅ２＋、Ｃｏ２＋、Ｎｉ２＋、Ｍｎ２＋、Ｚｎ２＋、Ｃｄ２＋、Ｃｕ２＋等均不迁移，故可以从这些离子的混合液中分离Ｎｄ（Ⅲ），其回收率达９４％以上。     

Recovery of neodymium,dysprosium,and cobalt from NdFeB magnet leachate using an unsymmetrical dialkylphosphinic acid extractant,INET-3

Rare earths (REs) and Co are critical strategic resources.Their recovery is crucial for ensuring that their supplies are adequate and for reducing environmental pollution.End-of-life NdFeB magnets are important secondary RE sources.The separation of Dy,Nd,and Co from NdFeB leachate using a relatively new extractant (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid (INET-3),was investigated in this study.The separation parameters,such as equilibrium pH,phase ratio,INET-3 concentration,and number of counter-current extraction stages,were optimised.The results show that INET-3 can separate Dy,Nd,and Co efficiently.For the preferential extraction of Dy from synthetic iron-free NdFeB leachate,the optimum equilibrium pH is 2.60.Under this condition,separation of Dy from the leachate requires four counter-current extraction stages at A/O (volume ratio of aqueous to organic)=1:2.This is demonstrated by a simulated four-stage counter-current extraction process.At equilibrium pH=2.52and A/O=1:2,98%of Dy is recovered with 95%purity.As to the subsequent separation of Nd from the leachate,nearly 100%is recovered with 99%purity through a simulated three-stage counter-current extraction process at equilibrium pH=5.33 and A/O=1:1.Approximately 95%of Co remains in the raffinate with 99.98%purity.     

从NdFeB磁性材料制造工业废料中提炼金属钕

综述了从ＮｄＦｅＢ生产的工业废料中提炼金属钕的生产工艺及生产工艺条件对产品质量、技术经济指标的影响。应用该工艺得到的金属钕成分特殊,重新用于ＮｄＦｅＢ合金熔炼,效益显著;从废料中提炼的具有特殊成分的氧化钕,用３０００Ａ电解槽生产,台日产金属钕６０ｋｇ,电流效率在于７５％,金属总收率大于８８％,生产工艺先进,成熟、稳定。     

Recycling rare earth from ultrafine NdFeB waste by capturing fluorine ions in wastewater and preparing them into nano-scale neodynium oxyfluoride

Ultrafine NdFeB waste is a relatively clean waste produced during NdFeB magnet processing. Fluorine-containing wastewater is a common type of industrial wastewater, such as stainless steel pickling wastewater. In this work, rare earth element neodynium was recycled from ultrafine NdFeB waste by capturing fluorine ions in the fluorine-containing wastewater and prepared into neodynium oxyfluoride. The reaction process was investigated through UV-Vis-NIR, thermogravimetry/differential thermogravimetry (TG/DTG), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The neodymium hydroxide in the ultrafine NdFeB waste reacted with fluorine ions to form Nd(OH)₂F, and Nd(OH)₂F was then transformed into neodymium oxyfluoride after decomposition. The formed neodymium oxyfluoride is found to be particles with rhombohedral structure and a particle size of around 50 nm. The reaction kinetics of forming Nd(OH)₂F was investigated. The reaction kinetic equation was established and the reaction activation energy was calculated. The effect of fluorine ion concentration on the reaction rate and products was evaluated. The results show that the reaction rate increases with the increase of fluorine ion concentration in the range of 0.01–1.5 mol/L, but it has little effect. In addition, the fluorine ion concentration affects the crystallinity of formed neodymium oxyfluoride. The recycling process not only realizes the sustainable utilization of rare earths, but also reduces the concentration of fluorine ions in the fluorine-containing wastewater, achieving two goals with one stone.     

Oxidative Roasting–Selective Pressure Leaching Process for Rare Earth Recovery from NdFeB Magnet Scrap

To recover rare earths (RE) with low acid consumption and low environmental pollution, selective pressure leaching with hydrochloric acid from roasted NdFeB scrap was explored. The phase evolution of NdFeB scrap during roasting at 800 °C as a function of time was confirmed, and after complete oxidation, its phase components consisted of Fe2O3, NdFeO3, and NdBO3. In the selective pressure leaching procedure, the optimal leaching was achieved at 110 °C for 30 min, in which the leaching rate of rare earth was 96.27% along with 13.33% of Fe. Subsequently, the effects of the hydrochloric acid dosage, the hydrochloric acid concentration and the particle size of the roasted NdFeB powder on the leaching rate of rare earth were investigated. For leaching at 110 °C for 30 min, the leaching of 13.33% Fe2O3 was derived from the Fe2O3 and NdFeO3 phases in the fully oxidized NdFeB scrap. This phenomenon was verified by the leaching of Fe from Fe2O3 of analytical purity and synthetic NdFeO3. Moreover, the leaching of Nd and Fe from the NdFeO3 phase was found to occur simultaneously. The advantages of the selective pressure leaching process using hydrochloric acid for the oxidized NdFeB scrap were comprehensively evaluated.     

Nd(III)在NaF-KF熔盐钨电极上电化学行为

钕铁硼磁体中稀土元素钕占据较大比重,从钕铁硼废料回收稀土有重大意义。为进一步了解钕在高温下氟化物熔盐的行为,本文在1 063 K采用NaF-KF(摩尔比2:3)电解质体系,加入质量分数为1%的NdF₃,以Pt为参比电极,钨棒为对电极,用循环伏安法等电化学暂态测试研究了Nd(III)在惰性钨电极上的电化学过程,探究Nd(III)的还原机理。结果显示:Nd(III)于NaF-KF-NdF₃熔盐中在惰性钨电极上的电化学还原过程是受扩散控制的不可逆的一步反应:Nd(III)+3e-=Nd,1 063 K时循环伏安法得到Nd(III)的扩散系数为2.107×10-5 cm2/s,钕的成核机制为瞬时成核。      

Study on Key Techniques for Producing High Performance NdFeB Sintered Permanent Magnets

ＮｄＦｅＢｍａｇｎｅｔｓｈａｖｅｂｅｅｎｉｍｐｒｏｖｅｄｄｒａ ｍａｔｉｃａｌｌｙｓｉｎｃｅｉｔｗａｓｉｎｖｅｎｔｅｄｉｎ 1 983 .Ｔｗｏｔｙｐｅｓｏｆｓｉｎｔｅｒｅｄｍａｇｎｅｔｓ ,ｈｉｇｈｅｎｅｒｇｙｐｒｏｄ ｕｃｔｓ ((ＢＨ ) ｍａｘ)ａｎｄｄｏｕｂｌｅｈｉｇｈ (ｈｉｇｈ(ＢＨ ) ｍａｘａｎｄｈｉｇｈｃｏｅｒｃｉｖｉｔｙ (ｉＨｃ) )ａｒｅｔｈｅｔｗｏｔｅｎｄｅｎｃｉｅｓｆｏｒＮｄＦｅＢｓｉｎｔｅｒｅｄｍａｇｎｅｔｓ .Ｂｏｔｈｆａｃｔｏｒｉｅｓａｎｄｒｅｓｅａｒｃｈｉｎｓｔｉｔｕｔｅｓａｒｅｆｏｃｕｓ…     

Characterization of Microstructure and Magnetic Properties of NdFeB Magnet with Dy, Al and Cu Additions

A new alloy of Nd33.5Dy0.99Febal.Al0.52Cu0.1B1.15 (%, mass fraction) was fabricated by powder metallurgy. The effects of Dy, Al and Cu additions on the microstructure and magnetic properties of sintered NdFeB magnet were investigated. The additions of Dy, Al and Cu are effective to refine grains and improve coercivity. Moreover, suitable amounts of Dy, Al and Cu lead to a demagnetization curve with good rectangularity. It is found that the sintered NdFeB magnet has relatively high magnetic performance of Br=12.17kGs, jHc=13.52kOe and (BH)max=34.71MGOe. The sintered NdFeB sample was examined by magnetic force microscope which revealed the domain structures at the surface. It is revealed that the mean Nd2Fe14B grain size is significantly larger than the average scale of the magnetic contrast. An explanation about this is that most Nd2Fe14B grains in sintered NdFeB alloy are dominated with the muhidomain structures when the magnet is in thermally demagnetization state.     

从钕铁硼废料中回收稀土及氧化钴的条件试验

研究了从钕铁硼废料中回收稀土氧化物和氧化钴的工艺流程,试验确定了酸分解,草酸沉淀,除铁等杂质的工艺条件,该工艺能有效地除去铁,钙等杂质,试验得到的氧化钴符合GB6518－86纯氧化钴粉Y1类产品要求,钴直收率在82％以上,所得稀土氧化物,其总含量为97％以上,回收率95％以上,达到了综合回收利用的目的。     

Effect of Cobalt on HDDR Anisotropic NdFeB

The effect of cobalt on the magnetic properties and anisotropy of HDDR anisotropic NdFeB was studied.It is found that Co is helpful for preparing anisotropic NdFeB with high coercivity. The research on the initial microstructure for NdFeB alloy indicates that Co tends to enter the crystal lattice of Nd-rich phase and some of Co atoms also enter the crystal lattice of Nd2Fe14B. The dissolution of Co changes the stability of Nd-rich phase and Nd2Fe14 B in H2 atmosphere and affects the kinetics of HDDR phase transformation. As a result, the NdFeB powder exhibits a high coercive force and a strong anisotropy.     

A Study of Grain Growth Kinetics in Sintered NdFeB Magnets

ＵｐｔｏｎｏｗｈｉｇｈｐｅｒｆｏｒｍａｎｃｅａｎｉｓｏｔｒｏｐｉｃＮｄＦｅＢ ｔｙｐｅｍａｇｎｅｔｓａｒｅｍａｉｎｌｙｍａｎｕｆａｃｔｕｒｅｄｂｙｔｈｅｐｏｗｄｅｒｍｅｔａｌｌｕｒｇｙｔｅｃｈｎｉｑｕｅ[1] .Ｔｈｅｆｉ ｎａｌｍｉｃｒｏｓｔｒｕｃｔｕｒｅｏｆｓｉｎｔｅｒｅｄＮｄＦｅＢｍａｇｎｅｔｓｉｓｄｅｔｅｒｍｉｎｅｄｂｙｔｈｅｐｒｅ ａｌｌｏｙｐｏｗｄｅｒｐａｒａｍｅ ｔｅｒｓａｎｄｓｉｎｔｅｒｉｎｇｃｏｎｄｉｔｉｏｎｓ .Ｔｈｅｔｅｃｈｎｏｌｏｇｉ ｃａｌｉｍｐｏｒｔａｎｃｅｏｆＮｄ2 Ｆｅ14 Ｂｇ…