基于碳骨架的多孔镍的制备与表征
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摘要
多孔镍具备多种优异物理性能如质轻、阻燃、很强的吸能本能和电磁屏蔽作用,而有着广泛的应用领域。本文通过扫描电镜、红外分析、容重法和万能材料拉伸实验机等分析测试手段研究碳骨架的表面预处理工艺和电镀液中加入不同分散剂时对沉积镍镀层组织和性能的影响规律。着重探讨了过硫酸铵和硫酸的浓度以及电镀液中分散剂对碳骨架表面形貌、沉积镍镀层形貌、压缩性能和容重等的影响规律与机制,以期获得制备多孔镍的最佳工艺条件。
研究结果表明：扩张粗化液中的过硫酸铵浓度小于200g/L时,所得到的碳骨架表面比较光洁,当过硫酸铵浓度大于250g/L时,碳骨架出现过腐蚀现象,随着过硫酸铵浓度增加,多孔镍的抗压强度增加,当过硫酸铵浓度为200g/L时多孔镍的抗压强度达到最高。当扩张粗化液中硫酸浓度小于100ml/L时,多孔镍的抗压强度变化不大,但是当其浓度大于100ml/L时,多孔镍的抗压强度明显降低。扩张粗化时间越长,碳骨架表面越粗糙,所得多孔镍的性能越好,但是超过40min时,性能明显下降。综合分析,确定碳骨架表面扩张粗化工艺为：过硫酸铵和硫酸的浓度分别为200g/L和100ml/L,扩张粗化时间为40min。
在柠檬酸钠、无水硫酸钠和硫酸镁三种分散剂中,采用柠檬酸钠制得的多孔镍镀层均匀,晶粒细小,表面光滑,力学性能最好。通过正交实验对比,得出了在硫酸盐体系中均镀能力很高的深孔镀镍工艺：镀液成分为NiSO4·7H2O 300 g/L；NiCl2·6H2O 40 g/L；硼酸40 g/L；十二烷基硫酸钠0.3g/L,糖精3g/L,温度为55℃,pH值为4.0)为柠檬酸钠浓度30g/L、电流密度为5mA/m2、时间为6h。其中,添加剂的引入大大促进了阴极极化,改善了镀液的性能,提高了均镀能力。在此工艺下,电沉积制备的多孔镍性能更好,孔隙率在85-90%,抗压强度达1.71MPa、弹性模量为0.054GPa。
通过正交实验对比,得出了在氨基磺酸盐体系中均镀能力很高的深孔镀镍工艺：镀液成分为氯化镍NiCl2·6H2O；5g/L,H3BO3：40g/L和十二烷基硫酸钠0.3g/L,镀液温度为55℃,pH值为4.1,氨基磺酸镍Ni(SO3NH2)2：550g/L、糖精4g/L、电流密度为5m A/m2、时间为9h。由最优制备工艺制备的多孔镍的抗压强度是16.3MPa、弹性模量为0.32GPa,孔隙率在80-90%。
Porous nickel is popular in a wide range of field because of its many excellent physical properties such as light mass, flame retardance, strong absorbed energy ability and electromagnetic shielding. The surface pretreatment technology of carbon skeleton and the law of effect about the structure and property of the nickel deposition when filling different dispersant into the electroplate bath was investigated and discussed. And the discussion is mainly about the concentration of the ammonium persulfate and sulphuric acid, and the influence and mechanism of the electroplating's dispersant to the surface of the carbon skeleton and nickel deposition coating. The compression characteristics and volume weight is also major point which the electroplating's dispersant affects. The target is getting the best technologcial conditions of the porous nickel's preparation.
As the reserch indicate:The surface of carbon skeleton will be more smooth, when chroma of ammonium persulfate in expansion coursed liquid is less than 200g/L, and when the chroma is more than 250g/L, the carbon skeleton will be over etching. Meanwhile the compression strength will increase as the adding of ammonium persulfate, and the compression strength will get to the biggest when the chroma is 200g/L. As for the chroma of sulfate in expansion coursed liquid, when it is less than 100mL/L, the compression. strength of porous nickel changed a little, but the strength will reduce obviously when the chroma is more than 100ml/L. Moreover, the property will goes better as the increasing of time and roughness of the surface of carbon skeleton A/m2.The intergrated ananysis indicates that the best technique of the expansion of rough of carbon skeleton is as follows: The chroma of ammonium deposition and sulfate is 200g/L, and the time of expansion of rough is 40min.
And the good porous nickel which is with even coating, fine grain, smooth surface and good mechanical property can be get when we use the sodium citrate as the dispersant which is better than anhydrous sodium sulfate and magnesium sulfate. from the conclusion of orthogonal experiments.The technics of electrodepositing foam were confirmed:NiSO4·7H2O 300g/L; NiCl2·6H2O 40g/L; H3PO440g/L; saccharin 3g/L; lauryl sodium sulfate 0.3g/L; the sodium citrate 30 g/L; pH 4.0; Current density 5 time of the mass of carbon skeleton A/m2; Temperature 55℃; the plating 6 hour.The plating abilities equally of plating liquid were improved by some additives worked in. Additives can make cathode more polarized and platingequally.At the same time,different additives were used in plating liquid together can improved the plating abilities of the liquid. Under this condition, foam metal had the better abilities,followed as:The porosity was 80-90%, the compressive strength was 1.71 MPa;theYoung'modulus was 0.054 GPa
From the conclusion of orthogonal experiments.The technics of electrodepositing foam were confirmed:Ni(SO3NH2)2:550g/L、; NiCl2·6H2O 5g/L; H3PO440g/L; saccharin 4g/L; lauryl sodium sulfate 0.3g/L; pH4.1; Current density 5 time of the mass of carbon skeleton; Temperature 55℃; the plating 9 hour. Under this condition, foam metal had the better abilities,followed as:The porosity was 80-90%, the compressive strength was 16.3MPa;theYoung'modulus was 0.32 GPa.
研究结果表明：扩张粗化液中的过硫酸铵浓度小于200g/L时,所得到的碳骨架表面比较光洁,当过硫酸铵浓度大于250g/L时,碳骨架出现过腐蚀现象,随着过硫酸铵浓度增加,多孔镍的抗压强度增加,当过硫酸铵浓度为200g/L时多孔镍的抗压强度达到最高。当扩张粗化液中硫酸浓度小于100ml/L时,多孔镍的抗压强度变化不大,但是当其浓度大于100ml/L时,多孔镍的抗压强度明显降低。扩张粗化时间越长,碳骨架表面越粗糙,所得多孔镍的性能越好,但是超过40min时,性能明显下降。综合分析,确定碳骨架表面扩张粗化工艺为：过硫酸铵和硫酸的浓度分别为200g/L和100ml/L,扩张粗化时间为40min。
在柠檬酸钠、无水硫酸钠和硫酸镁三种分散剂中,采用柠檬酸钠制得的多孔镍镀层均匀,晶粒细小,表面光滑,力学性能最好。通过正交实验对比,得出了在硫酸盐体系中均镀能力很高的深孔镀镍工艺：镀液成分为NiSO4·7H2O 300 g/L；NiCl2·6H2O 40 g/L；硼酸40 g/L；十二烷基硫酸钠0.3g/L,糖精3g/L,温度为55℃,pH值为4.0)为柠檬酸钠浓度30g/L、电流密度为5mA/m2、时间为6h。其中,添加剂的引入大大促进了阴极极化,改善了镀液的性能,提高了均镀能力。在此工艺下,电沉积制备的多孔镍性能更好,孔隙率在85-90%,抗压强度达1.71MPa、弹性模量为0.054GPa。
通过正交实验对比,得出了在氨基磺酸盐体系中均镀能力很高的深孔镀镍工艺：镀液成分为氯化镍NiCl2·6H2O；5g/L,H3BO3：40g/L和十二烷基硫酸钠0.3g/L,镀液温度为55℃,pH值为4.1,氨基磺酸镍Ni(SO3NH2)2：550g/L、糖精4g/L、电流密度为5m A/m2、时间为9h。由最优制备工艺制备的多孔镍的抗压强度是16.3MPa、弹性模量为0.32GPa,孔隙率在80-90%。
Porous nickel is popular in a wide range of field because of its many excellent physical properties such as light mass, flame retardance, strong absorbed energy ability and electromagnetic shielding. The surface pretreatment technology of carbon skeleton and the law of effect about the structure and property of the nickel deposition when filling different dispersant into the electroplate bath was investigated and discussed. And the discussion is mainly about the concentration of the ammonium persulfate and sulphuric acid, and the influence and mechanism of the electroplating's dispersant to the surface of the carbon skeleton and nickel deposition coating. The compression characteristics and volume weight is also major point which the electroplating's dispersant affects. The target is getting the best technologcial conditions of the porous nickel's preparation.
As the reserch indicate:The surface of carbon skeleton will be more smooth, when chroma of ammonium persulfate in expansion coursed liquid is less than 200g/L, and when the chroma is more than 250g/L, the carbon skeleton will be over etching. Meanwhile the compression strength will increase as the adding of ammonium persulfate, and the compression strength will get to the biggest when the chroma is 200g/L. As for the chroma of sulfate in expansion coursed liquid, when it is less than 100mL/L, the compression. strength of porous nickel changed a little, but the strength will reduce obviously when the chroma is more than 100ml/L. Moreover, the property will goes better as the increasing of time and roughness of the surface of carbon skeleton A/m2.The intergrated ananysis indicates that the best technique of the expansion of rough of carbon skeleton is as follows: The chroma of ammonium deposition and sulfate is 200g/L, and the time of expansion of rough is 40min.
And the good porous nickel which is with even coating, fine grain, smooth surface and good mechanical property can be get when we use the sodium citrate as the dispersant which is better than anhydrous sodium sulfate and magnesium sulfate. from the conclusion of orthogonal experiments.The technics of electrodepositing foam were confirmed:NiSO4·7H2O 300g/L; NiCl2·6H2O 40g/L; H3PO440g/L; saccharin 3g/L; lauryl sodium sulfate 0.3g/L; the sodium citrate 30 g/L; pH 4.0; Current density 5 time of the mass of carbon skeleton A/m2; Temperature 55℃; the plating 6 hour.The plating abilities equally of plating liquid were improved by some additives worked in. Additives can make cathode more polarized and platingequally.At the same time,different additives were used in plating liquid together can improved the plating abilities of the liquid. Under this condition, foam metal had the better abilities,followed as:The porosity was 80-90%, the compressive strength was 1.71 MPa;theYoung'modulus was 0.054 GPa
From the conclusion of orthogonal experiments.The technics of electrodepositing foam were confirmed:Ni(SO3NH2)2:550g/L、; NiCl2·6H2O 5g/L; H3PO440g/L; saccharin 4g/L; lauryl sodium sulfate 0.3g/L; pH4.1; Current density 5 time of the mass of carbon skeleton; Temperature 55℃; the plating 9 hour. Under this condition, foam metal had the better abilities,followed as:The porosity was 80-90%, the compressive strength was 16.3MPa;theYoung'modulus was 0.32 GPa.
引文
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