MSe_2（M=Nb，W）纳米材料的制备及摩擦学性能研究
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摘要
以MoS_2为代表的过渡族金属硫化物因其独特的层状结构,层间以范德华力结合,层内以很强的共价键结合,且在自然界中有大量矿藏,所以在摩擦领域得到了广泛的应用和研究。事实上,过渡族金属硒化物,如MSe_2(M=Nb,W)与MoS_2具有相似的物理结构及物理性质,将其作为润滑油添加剂添加到普通基础油中,可以明显的提高其减摩性能,但人们对其在摩擦领域的研究较少,因此我们利用固相合成法制备出了不同形貌的MSe_2(M=Nb,W)纳米材料,并对其在摩擦学性能方面的研究进行了探讨。
本文主要对过渡族金属硒化物MSe_2(M=Nb,W)型纳米材料的制备工艺和摩擦学性能等问题进行了初步探索。主要研究内容包括:
(1)将单质Nb粉和Se粉混合,密封在反应釜内,在高温管式炉中加热,通过固相反应合成了大量的NbSe_x微纳米片和纤维。对所合成的纳米材料分别用TEM、SEM、EDS、XRD等测试手段进行表面形貌和结构成分的表征。结果表明,提高温度有利于NbSe_x的结晶;温度较低时容易得到纤维状微纳米材料,直径100～300 nm,长度为几十微米;随着温度的升高,微纳米纤维逐渐消失而形成六边形状的片层结构,尺寸在10μm左右。
(2)将得到的NbSe_3纳米纤维进行高温分解,并利用SEM、EDS、TEM、HRTEM等测试手段对其产物进行了表面形貌和结构成分的表征。结果表明,得到了NbSe_2纳米纤维,直径150～300 nm,长度为几十微米。
(3)将单质W粉和Se粉密封在反应釜内,在高温管式炉中加热,通过固相反应合成了大量的WSe_2纳米片。对所合成的纳米材料分别用TEM、SEM、EDS、XRD等方法进行了结构、形貌和成分的测试和表征。结果表明,制备出的纳米材料具有纳米纤维,纳米片和纳米颗粒等不同形貌,其尺寸在100nm以内。
(4)将NbSe_x和WSe_2微纳米材料作为润滑油添加剂,在UMT-2摩擦磨损试验机上进行了不同条件的摩擦性能测试,对过渡族金属硒化物MSe_2(M=Nb,W)微纳米材料在边界润滑条件下的摩擦学行为进行了初步探讨,并对比了不同形貌的微纳米材料的摩擦学性能,结果表明,添加了纳米材料的润滑油的摩擦系数降低百分比为10%～30%。
(5)将NbSe_2微纳米材料与铜机械混合制备出了铜基复合材料并在UMT-2摩擦磨损试验机上对其进行了不同条件的摩擦性能测试,对NbSe_2微纳米材料在干摩擦条件下的摩擦学性能进行了研究,对比了不同形貌的NbSe_2微纳米材料对铜的摩擦学性能的影响。结果表明,添加了NbSe_2纳米材料的铜基复合材料具有更好的减摩性能。
(6)通过对添加纳米级固体添加剂的润滑油的摩擦性能试验,初步探讨了含有MSe_2(M=Nb,W)纳米级固体添加剂的润滑油的摩擦机制,其优异的摩擦性能可能归结于MSe_2纳米材料独特的结构,润滑膜机制和填充条件修复机制。
Recently,MoS_2 was studied widely in the field of friction due to its special layer structure,which is integrated by Van der Waals force between layers,while internal layer by strong covalent bond,and it is rich in mineral resources.As a matter of fact,transitional metal diselenium MSe_2 (M=Nb,W) has a similar physical structure and nature with MoS_2.It can be improve the friction reduction properties of base oil as lubricating oil additives,but there is less research about them in the field of friction.So MSe_2(M=Nb,W)nanomaterials were prepared by solid state reaction,and the tribological properties were also studied in this article.
In this paper,experimental investigation and theoretical analysis were carried out on the preparation process and tribological properties of transitional metal diselenium MSe_2(M=Nb,W) nanomaterials.
Firstly,NbSe_x(x=2,3) micro-nanomaterials were successfully prepared by solid-state reaction.The as-prepared products were characterized by X-ray diffraction(XRD),scanning electron microscopy (SEM),transmission electron microscopy(TEM),and high-resolution transmission electron microscopy(HRTEM).The results showed that it was helpful to NbSe_x crystallize to raise temperature,the fibers with diameter 100～300 nm and length several micometers could be obtained at lower temperature,and when temperature was raised the NbSe_x sheets were produced.
Secondly,NbSe_2 nanofibers were obtained from NbSe_3 nanofibers by high temperature decomposition.The as-obtained NbSe_2 nanofibers were characterized by EDS,scanning electron microscopy(SEM),TEM and HRTEM and so on.The results showed that the obtained fibers had a diameter 100～300 nm and length several tens of micometers.
Thirdly,WSe_2 nanomaterials were successfully prepared by solid-state reaction.The obtained products were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),and high-resolution transmission electron microscopy(HRTEM).The results showed that the obtained WSe_2 nano-materials had different morphology including nanofibers, nanosheets and nanoparticals,which grain size was about 100nm.
Fourthly,the tribological properties of NbSe_x and WSe_2 nanomaterials as lubricant additive were investigated on UMT-2 friction testing machine made in USA.And tests were carried on the condition of boundary lubrication and made a comparison on the tribological properties to the different morphology of NbSe_x nanomaterials.The results showed that friction coefficient of lubricants reduce percentage was 10%to 30%,as nanomaterials add into the base oil.
Fifthly,Copper-matrix composites were obtained by mechanical mixing the NbSe_2 nanomaterials and copper.The dry friction experiments of Cu-NbSe_2 composites were also carried on UMT-2 friction testing machine.And made a study of the effect on the tribological properties of Cu-NbSe_2 composites with different morphology.The results showed Cu-NbSe_2 composites had a better tribological properties
The last but not least,friction mechanism of transitional metal diselenium MSe_2(M=W,Nb) nanomaterials as lubricant and composites additive were discussed.The excellent tribological proerties of these nanomaterials may be due to the following factors:the special structures, the formationof lubrication films and fill up-repair mechanism.
本文主要对过渡族金属硒化物MSe_2(M=Nb,W)型纳米材料的制备工艺和摩擦学性能等问题进行了初步探索。主要研究内容包括:
(1)将单质Nb粉和Se粉混合,密封在反应釜内,在高温管式炉中加热,通过固相反应合成了大量的NbSe_x微纳米片和纤维。对所合成的纳米材料分别用TEM、SEM、EDS、XRD等测试手段进行表面形貌和结构成分的表征。结果表明,提高温度有利于NbSe_x的结晶;温度较低时容易得到纤维状微纳米材料,直径100～300 nm,长度为几十微米;随着温度的升高,微纳米纤维逐渐消失而形成六边形状的片层结构,尺寸在10μm左右。
(2)将得到的NbSe_3纳米纤维进行高温分解,并利用SEM、EDS、TEM、HRTEM等测试手段对其产物进行了表面形貌和结构成分的表征。结果表明,得到了NbSe_2纳米纤维,直径150～300 nm,长度为几十微米。
(3)将单质W粉和Se粉密封在反应釜内,在高温管式炉中加热,通过固相反应合成了大量的WSe_2纳米片。对所合成的纳米材料分别用TEM、SEM、EDS、XRD等方法进行了结构、形貌和成分的测试和表征。结果表明,制备出的纳米材料具有纳米纤维,纳米片和纳米颗粒等不同形貌,其尺寸在100nm以内。
(4)将NbSe_x和WSe_2微纳米材料作为润滑油添加剂,在UMT-2摩擦磨损试验机上进行了不同条件的摩擦性能测试,对过渡族金属硒化物MSe_2(M=Nb,W)微纳米材料在边界润滑条件下的摩擦学行为进行了初步探讨,并对比了不同形貌的微纳米材料的摩擦学性能,结果表明,添加了纳米材料的润滑油的摩擦系数降低百分比为10%～30%。
(5)将NbSe_2微纳米材料与铜机械混合制备出了铜基复合材料并在UMT-2摩擦磨损试验机上对其进行了不同条件的摩擦性能测试,对NbSe_2微纳米材料在干摩擦条件下的摩擦学性能进行了研究,对比了不同形貌的NbSe_2微纳米材料对铜的摩擦学性能的影响。结果表明,添加了NbSe_2纳米材料的铜基复合材料具有更好的减摩性能。
(6)通过对添加纳米级固体添加剂的润滑油的摩擦性能试验,初步探讨了含有MSe_2(M=Nb,W)纳米级固体添加剂的润滑油的摩擦机制,其优异的摩擦性能可能归结于MSe_2纳米材料独特的结构,润滑膜机制和填充条件修复机制。
Recently,MoS_2 was studied widely in the field of friction due to its special layer structure,which is integrated by Van der Waals force between layers,while internal layer by strong covalent bond,and it is rich in mineral resources.As a matter of fact,transitional metal diselenium MSe_2 (M=Nb,W) has a similar physical structure and nature with MoS_2.It can be improve the friction reduction properties of base oil as lubricating oil additives,but there is less research about them in the field of friction.So MSe_2(M=Nb,W)nanomaterials were prepared by solid state reaction,and the tribological properties were also studied in this article.
In this paper,experimental investigation and theoretical analysis were carried out on the preparation process and tribological properties of transitional metal diselenium MSe_2(M=Nb,W) nanomaterials.
Firstly,NbSe_x(x=2,3) micro-nanomaterials were successfully prepared by solid-state reaction.The as-prepared products were characterized by X-ray diffraction(XRD),scanning electron microscopy (SEM),transmission electron microscopy(TEM),and high-resolution transmission electron microscopy(HRTEM).The results showed that it was helpful to NbSe_x crystallize to raise temperature,the fibers with diameter 100～300 nm and length several micometers could be obtained at lower temperature,and when temperature was raised the NbSe_x sheets were produced.
Secondly,NbSe_2 nanofibers were obtained from NbSe_3 nanofibers by high temperature decomposition.The as-obtained NbSe_2 nanofibers were characterized by EDS,scanning electron microscopy(SEM),TEM and HRTEM and so on.The results showed that the obtained fibers had a diameter 100～300 nm and length several tens of micometers.
Thirdly,WSe_2 nanomaterials were successfully prepared by solid-state reaction.The obtained products were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),and high-resolution transmission electron microscopy(HRTEM).The results showed that the obtained WSe_2 nano-materials had different morphology including nanofibers, nanosheets and nanoparticals,which grain size was about 100nm.
Fourthly,the tribological properties of NbSe_x and WSe_2 nanomaterials as lubricant additive were investigated on UMT-2 friction testing machine made in USA.And tests were carried on the condition of boundary lubrication and made a comparison on the tribological properties to the different morphology of NbSe_x nanomaterials.The results showed that friction coefficient of lubricants reduce percentage was 10%to 30%,as nanomaterials add into the base oil.
Fifthly,Copper-matrix composites were obtained by mechanical mixing the NbSe_2 nanomaterials and copper.The dry friction experiments of Cu-NbSe_2 composites were also carried on UMT-2 friction testing machine.And made a study of the effect on the tribological properties of Cu-NbSe_2 composites with different morphology.The results showed Cu-NbSe_2 composites had a better tribological properties
The last but not least,friction mechanism of transitional metal diselenium MSe_2(M=W,Nb) nanomaterials as lubricant and composites additive were discussed.The excellent tribological proerties of these nanomaterials may be due to the following factors:the special structures, the formationof lubrication films and fill up-repair mechanism.
引文
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