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Effect of accelerators and stabilizers on the formation and characteristics of electroless Ni-P deposits

机译:促进剂和稳定剂对化学镀Ni-P沉积物的形成和特性的影响

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The effect of thiourea, succinic acid and lead acetate on the formation and characteristics of electroless Ni-P deposits obtained from an acidic hypophosphite reduced electroless nickel bath is addressed in this paper. The rate of deposition of electroless Ni-P coating is found to be a function of concentration of these additives. Thiourea accelerates the rate of deposition up to 0.8 ppm and started to inhibit at a concentration of I ppm. Similarly, succinic acid increases the plating rate up to 12 g l(-1) and exhibit an inhibiting effect at higher concentrations of the order of 15 g l(-1). Addition of lead acetate inhibits the rate of deposition even at a concentration of 0.5 ppm and the extent of inhibition is increased when the concentration is higher than I ppm. Addition of these additives also caused a change in phosphorus content of the deposits; lead acetate (1 ppm) tends to increase the phosphorus content whereas thiourea (0.8 ppm) and succinic acid (12 g l(-1)) tends to decrease the phosphorus content. The X-ray diffraction patterns of electroless Ni-P coatings obtained in the absence of additives and in presence of 1 ppm of lead acetate exhibit a single broad peak centered at 44.5 degrees 20, indicating the amorphous nature of these coatings. The peak broadening suggests a greater tendency to form amorphous structure when lead acetate is used as the additive. In contrast, for electroless Ni-P coatings obtained from thiourea and succinic acid containing baths, besides the reflection from Ni (1 1 1) plane, a weak reflection from Ni (2 0 0) plane is also observed. The X-ray diffraction patterns of electroless Ni-P coatings after annealing at 400 degrees C for 1 h exhibit the formation of fcc nickel and bct nickel phosphide (Ni3P) phases in all the cases with Ni3P (2 3 1) as the most intense reflection. Electroless Ni-P coatings obtained in presence of thiourea and succinic acid exhibit a nodular feature with a typical cauliflower like structure. The size of the nodules is relatively less in the latter case. In contrast, the electroless Ni-P coating obtained in the absence of additives and in presence of 1 ppm of lead acetate is relatively smooth. However, the deposit obtained in the absence of additives reveals the presence of fine particulates, attributed to the precipitation of MY phases in the absence of stabilizers. The DSC traces of electroless Ni-P coatings exhibit a single well-defined exothermic peak in the temperature range studied in all the cases, which could be attributed to the precipitation of metallic nickel phase and formation of nickel phosphide (Ni3P) phase. The variation in the peak temperature and the energy evolved during the phase transition is due to the slight variation in the phosphorus content caused by the addition of thiourea, succinic acid and lead acetate. The study recommends that the choice of accelerators and stabilizers should be made only after a careful study. (c) 2005 Elsevier B.V. All rights reserved.
机译:本文探讨了硫脲,琥珀酸和乙酸铅对从酸性次磷酸盐还原的化学镀镍浴中获得的化学镀Ni-P沉积物的形成和特性的影响。发现化学镀Ni-P涂层的沉积速率是这些添加剂的浓度的函数。硫脲将沉积速率提高到0.8 ppm,并在浓度为1 ppm时开始抑制。类似地,琥珀酸将电镀速率提高到12 g l(-1),并在15 g l(-1)的较高浓度下显示出抑制作用。乙酸铅的添加即使在0.5ppm的浓度下也抑制了沉积速率,并且当浓度高于1ppm时,抑制的程度增加了。这些添加剂的添加也导致沉积物中磷含量的变化;乙酸铅(1 ppm)倾向于增加磷含量,而硫脲(0.8 ppm)和琥珀酸(12 g l(-1))倾向于降低磷含量。在不存在添加剂和乙酸铅含量为1 ppm的情况下获得的化学镀Ni-P涂层的X射线衍射图谱显示出一个以44.5度20为中心的宽峰,表明这些涂层的非晶性。当使用乙酸铅作为添加剂时,峰展宽表明形成非晶结构的趋势更大。相反,对于从含硫脲和琥珀酸的浴中获得的化学镀Ni-P涂层,除了从Ni(1 1 1)平面反射,还观察到从Ni(2 0 0)平面反射。在所有情况下,以Ni3P(2 3 1)最强的情况下,化学镀Ni-P涂层在400摄氏度下退火1小时后的X射线衍射图显示fcc镍和bct磷化镍(Ni3P)相的形成。反射。在硫脲和琥珀酸存在下获得的化学镀Ni-P涂层呈现结节状特征,具有典型的菜花状结构。在后一种情况下,结节的大小相对较小。相反,在没有添加剂和乙酸铅为1ppm的情况下获得的化学镀Ni-P涂层是相对光滑的。然而,在不存在添加剂的情况下获得的沉积物显示存在细颗粒,这归因于在不存在稳定剂的情况下MY相的沉淀。在所有情况下研究的温度范围内,化学镀Ni-P涂层的DSC迹线都显示出一个明确定义的放热峰,这可能归因于金属镍相的沉淀和磷化镍(Ni3P)相的形成。峰值温度的变化和在相变过程中释放出的能量是由于添加硫脲,琥珀酸和乙酸铅引起的磷含量的轻微变化。研究建议仅在仔细研究后才能选择促进剂和稳定剂。 (c)2005 Elsevier B.V.保留所有权利。

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