金属钽电解抛光液的改进

为适应工业规模生产的需要,在现有几种金属钽电解抛光溶液的基础上,调整了电解液成分,调整后的电解液对钽丝抛光试验表明,抛光后丝材的线径均匀,表面达到光亮平整所需的时间较短,抛光过程中的电流、电压、也有明显下降,取得了较好的抛光效果。     

增材制造Inconel 718的电解质等离子体抛光工艺研究

为解决增材制造的镍基高温合金部件难以满足高性能航空构件表面质量的问题,采用电解质等离子体抛光技术对增材Inconel 718样件进行抛光工艺试验。基于部分析因和响应曲面分析法,研究了抛光电压、电解液温度、加工时间、抛光剂浓度和络合剂浓度对表面粗糙度和材料去除率的影响规律,并对加工参数组合进行望小优化。结果表明,当采用抛光电压314.4 V、电解液温度70℃、加工时间15 min、抛光剂和络合剂质量分数2%和2.5%,增材打印的Inconel 718工件表面粗糙度可从Ra2.93μm降至Ra0.307μm,此时的材料去除率为2.072μm/min。     

电化学抛光铜的实验研究

目的提高铜的表面质量,并将铜的去除量控制在适用范围,研究铜电化学抛光的溶液配比和最佳工艺参数。方法使用自行搭建的电化学抛光系统对工件进行电化学抛光,并使用3D表面轮廓仪和精密电子天平测量工件加工前后的表面粗糙度和质量。采用单因素和正交实验结合的方法设计了实验方案,研究了磷酸浓度、电解液温度、电压、占空比、频率和加工时间对铜表面粗糙度的影响,以及添加剂对实验结果的影响。结果得到磷酸浓度和温度对表面粗糙度的影响曲线。通过极差分析得到了电压、占空比、频率和加工时间对表面粗糙度的影响趋势以及最优参数。在溶液中加入抗坏血酸后,材料去除率可以降低到1000 nm/min以下,但表面粗糙度最高达到75 nm。同时加入抗坏血酸和乙烯硫脲后,材料去除率为400 nm/min,表面粗糙度最低达到17 nm。结论电化学抛光铜的最优参数为:电压10 V,占空比23%,频率23 k Hz,加工时间11~14 min,溶液配比为55%磷酸+0.3%抗坏血酸+0.2%乙烯硫脲。抗坏血酸可以有效地控制材料去除率,抗坏血酸与乙烯硫脲同时作用又可以降低铜的表面粗糙度。     

钛合金结构件磁流变电解复合抛光试验研究

目的 针对钛合金结构件高质高效抛光需求，提出了磁流变电解复合抛光新方法，探究不同抛光参数对钛合金表面质量的影响，以实现钛合金构件的高质高效抛光。方法 深入探究了加工电压、加工间隙、电解质质量分数和抛光转速等参数对钛合金抛光表面粗糙度以及粗糙度变化率的影响，分析了不同抛光参数下的钛合金表面形貌变化，验证了磁流变电解复合抛光钛合金的可行性。结果 随着电解液中Na NO3质量分数的提高，钛合金表面粗糙度先减小后增大，质量分数为1.0%～2.5%时，得到了优于单磁流变抛光加工的抛光效果。不同加工电压下的表面粗糙度对比结果表明，在加工电压为0.1 V时，钛合金加工后表面粗糙度达到最小，而后随着加工电压的增大，加工区域表面粗糙度呈现增大趋势；随着加工间隙的增大，钛合金抛光表面粗糙度呈现先减小后增大的趋势；随着抛光工具转速增大，钛合金加工后表面粗糙度先减小后增大。相比于单一的磁流变抛光，磁流变电解复合抛光钛合金90 min，可使表面粗糙度从初始323 nm降低至15nm，加工效率提高了62.5%。结论 磁流变电解复合抛光工艺能够用于钛合金人工关节假体高效高质量的抛光。     

SLM零件的磨粒流动辅助电化学复合抛光方法研究

针对增材制造金属零件表面质量较差的问题，提出一种磨粒流动辅助电化学复合抛光方法，在电解液中混入微小磨粒，使混合液在一定压力下流经工件表面，通过磨粒磨削和电化学溶解的复合作用改善工件表面质量。通过试验对比了纯磨粒磨削、纯电解加工和复合抛光的加工效果，分析了不同工艺参数对工件表面粗糙度和材料去除量的影响。试验结果表明：复合抛光方法能有效去除增材制造零件表面缺陷，改善其表面质量。通过选取合适的电压进行分阶段抛光，SLM工件的表面粗糙度由Ra8.162μm降至Ra1.226μm。     

304钢等离子体电解抛光工艺与其表面结构性能研究

目的 减小304钢的表面粗糙度,以满足工程应用中对高质量表面的需求。方法 提出采用等离子体电解抛光(Plasma Electrolytic Polishing,PEP)技术实现304钢表面精整改性,结合高速摄影技术,研究等离子体电解抛光放电过程。通过对比304钢在不同电解液中形成钝化膜的电化学特性,探究不同工艺参数对抛光效果的影响,进一步设计正交试验研究不同因素间的交互作用及最佳工艺方案,阐释抛光前后表面微观形貌与浸润性、耐腐蚀性能及硬度的关系。结果 通过对比分析不同电解液体系中304钢表面钝化膜的电化学特性表明,304钢在(NH4)2SO4溶液中的腐蚀电位最低,钝化膜更容易被击穿,因此选用(NH4)2SO4作为电解液。正交试验和极差分析结果表明,304钢在抛光电压370 V、电解液温度80 ℃、电解质质量分数7%、抛光时间6 min的条件下获得最小的粗糙度(~0.050 mm)。各因素对304钢表面粗糙度的影响大小顺序为电解液温度>抛光时间>抛光电压>电解质浓度。表面性能结果显示,抛光后304钢的表面光洁度显著提高,呈镜面光泽,接触角由35.09°提升至78.52°,耐腐蚀性有所提高,表面硬度略有下降。结论 通过等离子体电解抛光实现304钢表面粗糙度减小及表面质量的显著提高,该技术具有抛光效率高、工艺简单、节能环保等优点,可广泛应用于生物医疗、石油化工、机械制造等领域。     

钽、铌及其合金金相样品制备方法

钽、铌及其合金具有很好的延性。磨制金相试样时微细磨痕难以去除且易变形产生冷作硬化层,影响真实组织的显示。为了得到光滑、平整、无冷作硬化层的金相磨面,曾做了许多研究工作。W.D.Forgeng研究了钽、铌的机械-化学抛光法、腐蚀抛光法及电解抛光法。GEORG、BLANN介绍了铌的电解-机械抛光法。近几年用高氯酸镁-甲醇低温电解液抛     

碳化硅晶体电化学机械抛光工艺研究

针对碳化硅晶体抛光效率低的问题,研究碳化硅晶体的电化学机械抛光工艺,对比NaOH、NaNO₃、H₃PO₄ 3种电解液电化学氧化碳化硅晶体的效果。选用0.6 mol/L的NaNO₃作为电化学机械抛光过程的电解液,使用金刚石–氧化铝混合磨粒,通过正交试验研究载荷、转速、电压、磨粒粒径对电化学机械抛光碳化硅晶体的表面质量和材料去除率的影响。采用优选的试验参数进行抛光试验,结果表明:在粗抛阶段可实现20.259 μm/h的高效材料去除,在精密抛光阶段可获得碳化硅表面粗糙度S_a为0.408 nm的光滑表面。      

高速磨粒流动辅助电解复合加工方法

针对难加工材料表面抛光难、工具损耗严重、加工效率低的问题,提出了一种高速磨粒流动辅助电解加工的方法,通过在电解液中添加微小磨粒,伴随电解液高速流动实现电化学溶解与钝化膜微量磨削的复合加工。针对该方法的加工参数进行了分析,研究了加工时间、加工电压、加工间隙、电解液浓度、电源种类、磨粒粒径对实验结果的影响。结果表明:采用5 V电压的直流电源,以质量分数10%的NaNO3作为电解液,设定加工间隙1 mm,用1200目的磨粒加工5 min,可得到表面质量较好的工件,表面粗糙度Ra<0.1μm。     

高效高质量加工特种钢的复合电解液试验研究

为实现S-03特种钢的高效、高表面质量电解加工,采用正交与灰关联理论相结合的方法,先进行了Na NO3、Na Cl O3电解液预试验研究,分析了电压和进给速度对材料去除率、表面粗糙度及侧面间隙的影响规律。为进一步提高加工效率,在复合电解液中添加Na Cl,研究电流密度对表面粗糙度的影响规律。结果表明:采用质量分数5%Na Cl+16%Na NO3+4%Na Cl O3的复合电解液,在电压24 V、电解液压力0.8 MPa、电解液温度30~35℃的条件下,实现了进给速度2.4 mm/min、表面粗糙度Ra0.4μm的高效、高表面质量加工。     

Flake tantalum powder for manufacturing electrolytic capacitors

The FTP200 flake tantalum powder was introduced.The microstructures of the powder with leaf-like primary particles having an average flakiness of 2 to 20 and porous agglomerated particles were observed.The chemical composition,physical properties,and electrical properties of the FTP200 powder were compared with those of the FTW300 nodular powder.The FTP200 powder is more sinter-resistant,and the surface area of the flake tantalum powder under sintering at high temperature has less loss than that of the nodular tantalum powder.The specific capacitance of the flake tantalum powder is higher than that of the nodular tantalum powder with the same surface area when anodized at high voltage.Thus,the flake tantalum powder is suitable for manufacturing tantalum solid electrolytic capacitors in the range of median and high（20-63 V） voltages.     

钽表面微弧氧化陶瓷层的制备及耐磨性能研究

目的研究不同电压、电流和氧化时间下,钽表面微弧氧化陶瓷层的生长机理与耐磨性能的变化。方法通过微弧氧化技术在钽金属表面制备陶瓷层,并采用扫描电子显微镜观察陶瓷层的表面形貌,采用摩擦磨损试验仪对陶瓷层的摩擦学性能进行研究,探讨放电电压、放电频率、氧化时间对陶瓷层摩擦系数的影响。结果在电压400 V、频率1000 Hz、氧化时间20 min条件下获得的陶瓷层表面质量最好;在电压350 V,频率1000 Hz,氧化时间10 min条件下获得的陶瓷层耐摩擦性能最好。结论对钽金属表面进行微弧氧化处理,可以显著降低钽金属表面的摩擦系数,提高耐磨性能。     

Electrochemical behavior of tantalum in ethylene carbonate and aluminum chloride solvate ionic liquid

To investigate the electrochemical reduction mechanism of Ta(V) in ethylene carbonate and aluminum chloride (EC−AlCl₃) solvate ionic liquid, cyclic voltammetry experiments were conducted on a tungsten working electrode. Four reduction peaks were observed in the cyclic voltammogram of the EC−AlCl₃−TaCl₅ ionic liquid. The reduction peaks at −0.55, −0.72, and −1.12 V (vs Al) were related to the reduction of Ta(V) to tantalum metal by three stages including the formation of Ta(IV) and Ta(III) complex ions. The reduction of Ta(III) to tantalum metal was an irreversible diffusion-controlled reaction with a diffusion coefficient of 3.7×10⁻⁷ cm²/s at 323 K, and the diffusion activation energy was 77 kJ/mol. Moreover, the cathode products at 323 K were characterized by scanning electron microscopy, energy-dispersive spectroscopy, and X-ray photoelectron spectroscopy. The results showed that tantalum metal and tantalum oxides were obtained by potentiostatic electrodeposition at −0.8 V for 2 h.     

Ag和Ta离子双注入Ti6Al4V合金表面改性

采用先注入1×1017ion/cm2Ag离子,注入能量为64.2keV;后注入1.5×1017ion/cm2Ta离子,注入能量为146.5keV对Ti6Al4V合金进行离子双注入表面改性。采用X射线衍射分析离子双注入前后Ti6Al4V合金表面的物相;利用X射线光电子能谱研究离子双注入前后Ti6Al4V合金表面元素化合态以及离子双注入Ti6Al4V合金表面元素浓度沿深度方向的分布。结果表明,离子双注入前后Ti6Al4V合金表面都被氧化了,离子注入前合金表面存在TiO、Ti2O3和Al2O3,离子双注入后Ti6Al4V合金表面有TiO2、Ta2O5、TaOx和AgO2新相生成,且在表面还存在少量V2O5和Al2O3。离子双注入合金表面生成的氧化物层形成了扩散阻挡层,阻挡铝离子和钒离子向外扩散,从而减少Ti6Al4V合金表面铝离子和钒离子的释放量。     

钽涂层多孔钛合金支架的制备与表征

钽金属是一种理想的医用金属材料,能够与人体软/硬组织发生整合。利用化学气相沉积方法,在可控多孔结构的Ti6Al4V合金支架表面沉积涂覆钽金属涂层,使其同时具备理想的三维孔隙结构和力学相容性,以及钽金属优异的生物学性能。研究结果显示,多孔钛合金支架表面涂层前后色泽发生明显变化,涂层后支架呈现钽金属色泽。扫描电镜和XRD分析进一步证明了多孔钛合金支架表面沉积物为钽金属。与美国Zimmer公司生产的多孔钽小梁金属相比,钽涂层多孔钛合金支架具备与人体皮质骨更相似的弹性模量和抗压强度,是一种理想的骨修复替代物。     

Phase evolution of tantalum nitride and tantalum carbide films with PBII parameters

Tantalum nitride and tantalum carbide films were fabricated using magnetron sputtering of tantalum followed by nitrogen and carbon plasma-based ion implantation (N-PBII and C-PBII). The phase evolution and morphology of the films were studied using glancing angle X-ray diffraction (GXRD) and transmission electron microscopy (TEM). It was found that the main phase in the tantalum nitride films was crystalline TaN_0.1 whose grain size increases with increasing implantation voltage and phase content increases with increasing implantation dose. In the tantalum carbide film, the main phase was Ta₂C. TaC phase also appeared as the implantation dose increased. XRD results from various glancing angles show that the phases with high nitrogen or carbon content, Ta₄N₅ and TaC, are present in the surface of the films. X-ray photoelectron spectra (XPS) from the tantalum carbide film reveal that the surface carbon content is higher than that of the inner film.     

Preparation of high-purity tantalum ethoxide by vacuum distillation

Effects of reflux ratio, water addition and content of water in ethanol on the purity and yield of tantalum ethoxide during vacuum distillation were investigated under the operational conditions of pressure of 1kPa, oil bath temperature of 210-230 ℃, and outlet temperature of 190℃. The condensate sample was characterized by FTIR, 1↑H-NMR spectroscopy and Raman spectra, respectively. The contents of tantalum, carbon and hydrogen in the sample were also determined with elemental analysis instrument. The obtained results consistently demonstrate that the condensate is tantalum ethoxide. The content of impurity, such as Al, As, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Ni, Pb, Sn, Ti, V and Zn, in tantalum ethoxide is less than 0.000 05%, while Nb content is less than 0.000 5%. The content of impurities in tantalum ethoxide sample excels that of Epichem Group＇s requirement for Ta（OC2H5）5 of 99.999%.     

Corrosion rate of construction materials in hot phosphoric acid with the contribution of anodic polarization

The paper is focused on selection of a proper material for construction elements of water electrolysers, which make use of a 85% phosphoric acid as an electrolyte at temperature of 150 °C and which might be loaded with anodic polarization up to 2.5 V versus a saturated Ag/AgCl electrode (SSCE). Several grades of stainless steels were tested as well as tantalum, niobium, titanium, nickel alloys and silicon carbide. The corrosion rate was evaluated by means of mass loss at free corrosion potential as well as under various levels of polarization. The only corrosion resistant material in 85% phosphoric acid at 150 °C and at polarization of 2.5 V/SSCE is tantalum. In that case, even a gentle cathodic polarization is harmful in such an acidic environment. Hydrogen reduction leads to tantalum hydride formation, to loss of mechanical properties and to complete disintegration of the metal. Contrary to tantalum, titanium is free of any corrosion resistance in hot phosphoric acid. Its corrosion rate ranges from tens of millimetres to metres per year depending on temperature of the acid. Alloy bonded tantalum coating was recognized as an effective corrosion protection for both titanium and stainless steel. Its serviceability might be limited by slow dissolution of tantalum that is in order of units of mm/year.     

基于Ti-5Al-1V-1SN-1Zr-0.8Mo合金的分段电压微弧氧化膜层的研究

本文主要研究分段电压对于钛合金表面所制备的微弧氧化膜层特性的影响。利用扫描电子显微镜(SEM)和激光扫描共聚焦显微镜对MAO膜层的结构进行了表征,利用能谱分析(EDS)和X射线衍射(XRD)并对膜层成分进行分析。对比评价了不同分段电压模式下膜层的厚度、粗糙度和耐蚀性。结果表明,与不同分段电压相比,第一阶段电压为320V 氧化时间180s与第二阶段电压为420V氧化时间为720s,所形成的膜层粗糙度最小。第一阶段外加电压320V氧化时间120s与第二阶段外加电压420V时间780s,膜层最为致密,耐腐蚀性最好。XRD结果表明,膜层是由TiO2和亚稳态Ti2O3组成。     

钽等离子体渗氮的表面过程分析

对钽表面渗氮的固－气界面反应过程进行了热力学和动力学分析,从到理论预测了各种参数（压力、气体、组成、温度、电参数等）对表面过程的影响,并借助于等离子体,在较你廿获得由层与Ｎ在ＴＡ中的固溶体组成的表面硬化层,层为六方晶系的Ｔａ６Ｎ２,５７和／或非昌态。通过调整工艺参数有效地抑制了钽表面氧的渗入和Ｔａ２Ｏ５的形成,使得离子渗氮后,仍保持较低的表面粗糙度。