石墨烯及石墨烯基铜/碳核壳结构材料的制备和场发射性能的研究
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摘要
石墨烯是由一个sp~2杂化碳原子层构成的二维蜂窝状晶格结构材料，由于其特殊的结构和优异的物理性能，如大的比表面积、高的电子迁移率、好的化学稳定性及良好的柔韧性等，使石墨烯及石墨烯基复合材料在电子及光电子器件、化学传感器和能量储存器件等领域具有广泛的应用前景。
在众多的制备石墨烯的方法中，化学气相沉积（CVD）方法是制备大面积、高品质石墨烯的最有效方法之一，然而，这种方法需要极高的反应温度和较多的碳源。对于等离子体增强化学气相沉积（PECVD）方法来说，它是目前用于沉积各种碳材料、半导体材料的较为普遍使用的方法，这种沉积技术借助于辉光放电使碳源气体发生分解，最终含有薄膜组分的活性基团发生化学反应，从而实现薄膜材料的生长。可见，利用PECVD方法可以在反应温度相对较低、沉积时间较短、所需碳源较少的条件下制备石墨烯，大大地降低了石墨烯的制备成本。本论文采用射频等离子体增强化学气相沉积（RF-PECVD）设备，以多晶钴薄膜为生长基底，通过合理地控制钴薄膜的厚度、基底的温度和沉积的时间，制备了高品质的石墨烯，同时，结合第一性原理密度泛函理论计算探讨了石墨烯的生长机制。
石墨烯具有极好的化学稳定性，可以作为金属颗粒（如：钴、镍和铜等）的保护壳层，因此，近些年越来越多的科研工作者致力于寻找一种简单而有效的方法来制备金属/碳的核壳结构材料。本论文使用RF-PECVD设备，通过合理的控制沉积时间成功地获得了一种新型的石墨烯基铜/碳核壳结构材料，并详细地探讨了其生长机制。
石墨烯由于其具有优异的电子输运性质和良好的导热性能，有望应用于场发射器件的电极材料。本论文系统地研究了铜颗粒的尺寸及颗粒之间的距离对新型核壳结构材料的场发射性能的影响，并重点探讨了该核壳结构材料的场发射增强机制，为石墨烯基材料作为场发射器件的电极材料奠定了研究基础。
Graphene is a two-dimensional honeycomb lattice material bonded with a singlelayer of sp~2-hybridized carbon atoms, exhibiting excellent physical properties,including extremely high electronic mobility, thermodynamic stability, great elasticity,etc. Since graphene was obtained by Geim and Novoselov using a mechanicalexfoliation method in2004, great interest has been attracted to synthesize and exploreits potential applications in the fields of field-effect transistors, vapor sensors,batteries, supercapacitors and biosensors. In recent years, although great process hasbeen made on graphene by theoretical and experimental studies, further investigationsneed to be done on both preparation and application of graphene, such as how toreduce the cost of the preparation of graphene, what is the growth mechanism ofgraphene, how to modulate the morphology and structure of graphene, whether theproperties of graphene-based composite materials could be developed or improved?Based on these issues, the main research contents and the important results of thisdissertation are summarized as follows:
In Chapter2, one to five layer graphene have been successfully prepared on apolycrystalline Co film at a relatively low temperature (800℃) and a slow total gasflow rate (78sccm) for40s by RF-PECVD technique, which has efficiently reducedthe preparation cost of graphene. Furthermore, the graphene exhibits a high opticaltransmittance of more than70%in the wavelength range500–1200nm and has asheet resistivity of2.661kΩ/sq. thickness of Co film, substrate temperature and deposition time on the growth ofgraphene. When the thickness of Co film is increased from300nm to600nm, the Cofilm becomes more continuous at800℃, which is favor to form graphene with highquality. When the substrate temperature is changed from800℃to700℃, the activityof polycrystalline Co surface decreases and the diffusion rate of carbon atoms on Cosurface becomes slower, which will cause a decline of growth rate of graphene. Thus,the quality of graphene decreases greatly. When the deposition time is increased, thequality of graphene changes greatly. Finally, we conclude that the graphenesynthesized by40s are most uniform and has the largest in-plane crystallite sizeaccording to the I2D/IGand FWHM2Dvalue. Based on the first-principles densityfunctional theorical (DFT) results, the barriers for carbon atoms penetrating from thesubsurface octahedral sites of Co (111) to the surface is extremely higher than thatdiffusing on the surface, suggesting that the graphene is more easily formed by asurface direct growth process.
In Chapter4, a novel hedgehog-like core/shell structure, consisting of a highdensity of vertically aligned graphene sheets and a thin graphene shell/a copper core(VGs-GS/CC), has been synthesized using RF-PECVD. A Cu film with a thickness ofabout120nm deposited on Si (100) wafer by direct current magnetron sputtering wasused as Cu source. The growth mechanism of VGs-GS/CC is discussed. It is knownthat Cu has a relative low carbon solubility (0.04at%at1085℃) and the carbondissolved in the Cu particles will become supersaturated under a relative longdeposition time. Then, graphene sheets begin to nucleate and grow up on Cu surface.At an initial state, nucleation sites are enlarged along two-dimensional direction onCu surface. When two growing graphene sheets meet each other, graphene sheets areforced to rise upwards, causing the formation of vertically aligned graphene sheets(VGs). In the process of cooling, carbon atoms segregate from the interior of Cuparticles to form graphene layers at the interlayer between Cu and VGs. Consequently,VGs-GS/CC material is obtained. In addition, we find that VGs-GS/CC materialexhibits an improved field emission property, compared to VGs grown on Si substrate. This can be attributed to the geometrical factors such as a high density of emitters(more sharp edges) on Cu particles and the randomly distribution of VGs-GS/CC onSi substrate. Hence,‘field shielding’ effect among VGs is weakened and VGs-GS/CCmaterial exhibits an improved FE property.
In Chapter5, Cu films with a thickness of6,12,36,60and120nm are depositedon Si (100) wafers by using direct current magnetron sputtering. They are used as Cusource to synthesize VGs-GS/CC_6, VGs-GS/CC_12, VGs-GS/CC_36, VGs-GS/CC_60andVGs-GS/CC120via RF-PECVD. Field emission measurements show that theVGs-GS/CC_6hybrid material has the lowest turn-on field (2.4V/μm) at a currentdensity of1μA/cm2and exhibits the largest field enhancement factor (~6450), whichis about4.9times higher than that of VGs on Si. The enhanced field emissionproperties of VGs-GS/CC are attributed to not only the high conduction of Cu, butalso the geometrical factors of Cu particles such as particle size and inter-particledistance:
(1) In the high-field region where E>5.6V/μm, the current density is directlyproportional to the percentage of Cu particles within a size range of75–125nm forthe VGs-GS/CC samples. VGs on Cu particles within a small diameter of75–125nm like convex films, causing the area density of VGs on Cu particles decreased.Under a less screening from neighboring VGs, the emitting efficiency becomesgreatly enhanced.
(2) In the low-field region where2.1 In conclusion, high-quality, few-layer graphene has been successfully preparedvia RF-PECVD on a polycrystalline Co film. The thickness of Co film, the substratetemperature and the deposition time play important roles in the graphene growth.Based on the first-principles density functional theorical (DFT) results, we find that graphene is more easily formed by a surface direct growth process. Theseinvestigations will give a helpful guidance in synthesis and practical application ofgraphene. In addition, we have successfully synthesized a novel hedgehog-likecore/shell structure (VGs-GS/CC) using RF-PECVD. And field emissionmeasurement shows that the VGs-GS/CC exhibits better field emission performancethan VGs/Si, which suggests that the VGs-GS/CC materials are good candidates forfield emitters.
在众多的制备石墨烯的方法中，化学气相沉积（CVD）方法是制备大面积、高品质石墨烯的最有效方法之一，然而，这种方法需要极高的反应温度和较多的碳源。对于等离子体增强化学气相沉积（PECVD）方法来说，它是目前用于沉积各种碳材料、半导体材料的较为普遍使用的方法，这种沉积技术借助于辉光放电使碳源气体发生分解，最终含有薄膜组分的活性基团发生化学反应，从而实现薄膜材料的生长。可见，利用PECVD方法可以在反应温度相对较低、沉积时间较短、所需碳源较少的条件下制备石墨烯，大大地降低了石墨烯的制备成本。本论文采用射频等离子体增强化学气相沉积（RF-PECVD）设备，以多晶钴薄膜为生长基底，通过合理地控制钴薄膜的厚度、基底的温度和沉积的时间，制备了高品质的石墨烯，同时，结合第一性原理密度泛函理论计算探讨了石墨烯的生长机制。
石墨烯具有极好的化学稳定性，可以作为金属颗粒（如：钴、镍和铜等）的保护壳层，因此，近些年越来越多的科研工作者致力于寻找一种简单而有效的方法来制备金属/碳的核壳结构材料。本论文使用RF-PECVD设备，通过合理的控制沉积时间成功地获得了一种新型的石墨烯基铜/碳核壳结构材料，并详细地探讨了其生长机制。
石墨烯由于其具有优异的电子输运性质和良好的导热性能，有望应用于场发射器件的电极材料。本论文系统地研究了铜颗粒的尺寸及颗粒之间的距离对新型核壳结构材料的场发射性能的影响，并重点探讨了该核壳结构材料的场发射增强机制，为石墨烯基材料作为场发射器件的电极材料奠定了研究基础。
Graphene is a two-dimensional honeycomb lattice material bonded with a singlelayer of sp~2-hybridized carbon atoms, exhibiting excellent physical properties,including extremely high electronic mobility, thermodynamic stability, great elasticity,etc. Since graphene was obtained by Geim and Novoselov using a mechanicalexfoliation method in2004, great interest has been attracted to synthesize and exploreits potential applications in the fields of field-effect transistors, vapor sensors,batteries, supercapacitors and biosensors. In recent years, although great process hasbeen made on graphene by theoretical and experimental studies, further investigationsneed to be done on both preparation and application of graphene, such as how toreduce the cost of the preparation of graphene, what is the growth mechanism ofgraphene, how to modulate the morphology and structure of graphene, whether theproperties of graphene-based composite materials could be developed or improved?Based on these issues, the main research contents and the important results of thisdissertation are summarized as follows:
In Chapter2, one to five layer graphene have been successfully prepared on apolycrystalline Co film at a relatively low temperature (800℃) and a slow total gasflow rate (78sccm) for40s by RF-PECVD technique, which has efficiently reducedthe preparation cost of graphene. Furthermore, the graphene exhibits a high opticaltransmittance of more than70%in the wavelength range500–1200nm and has asheet resistivity of2.661kΩ/sq. thickness of Co film, substrate temperature and deposition time on the growth ofgraphene. When the thickness of Co film is increased from300nm to600nm, the Cofilm becomes more continuous at800℃, which is favor to form graphene with highquality. When the substrate temperature is changed from800℃to700℃, the activityof polycrystalline Co surface decreases and the diffusion rate of carbon atoms on Cosurface becomes slower, which will cause a decline of growth rate of graphene. Thus,the quality of graphene decreases greatly. When the deposition time is increased, thequality of graphene changes greatly. Finally, we conclude that the graphenesynthesized by40s are most uniform and has the largest in-plane crystallite sizeaccording to the I2D/IGand FWHM2Dvalue. Based on the first-principles densityfunctional theorical (DFT) results, the barriers for carbon atoms penetrating from thesubsurface octahedral sites of Co (111) to the surface is extremely higher than thatdiffusing on the surface, suggesting that the graphene is more easily formed by asurface direct growth process.
In Chapter4, a novel hedgehog-like core/shell structure, consisting of a highdensity of vertically aligned graphene sheets and a thin graphene shell/a copper core(VGs-GS/CC), has been synthesized using RF-PECVD. A Cu film with a thickness ofabout120nm deposited on Si (100) wafer by direct current magnetron sputtering wasused as Cu source. The growth mechanism of VGs-GS/CC is discussed. It is knownthat Cu has a relative low carbon solubility (0.04at%at1085℃) and the carbondissolved in the Cu particles will become supersaturated under a relative longdeposition time. Then, graphene sheets begin to nucleate and grow up on Cu surface.At an initial state, nucleation sites are enlarged along two-dimensional direction onCu surface. When two growing graphene sheets meet each other, graphene sheets areforced to rise upwards, causing the formation of vertically aligned graphene sheets(VGs). In the process of cooling, carbon atoms segregate from the interior of Cuparticles to form graphene layers at the interlayer between Cu and VGs. Consequently,VGs-GS/CC material is obtained. In addition, we find that VGs-GS/CC materialexhibits an improved field emission property, compared to VGs grown on Si substrate. This can be attributed to the geometrical factors such as a high density of emitters(more sharp edges) on Cu particles and the randomly distribution of VGs-GS/CC onSi substrate. Hence,‘field shielding’ effect among VGs is weakened and VGs-GS/CCmaterial exhibits an improved FE property.
In Chapter5, Cu films with a thickness of6,12,36,60and120nm are depositedon Si (100) wafers by using direct current magnetron sputtering. They are used as Cusource to synthesize VGs-GS/CC_6, VGs-GS/CC_12, VGs-GS/CC_36, VGs-GS/CC_60andVGs-GS/CC120via RF-PECVD. Field emission measurements show that theVGs-GS/CC_6hybrid material has the lowest turn-on field (2.4V/μm) at a currentdensity of1μA/cm2and exhibits the largest field enhancement factor (~6450), whichis about4.9times higher than that of VGs on Si. The enhanced field emissionproperties of VGs-GS/CC are attributed to not only the high conduction of Cu, butalso the geometrical factors of Cu particles such as particle size and inter-particledistance:
(1) In the high-field region where E>5.6V/μm, the current density is directlyproportional to the percentage of Cu particles within a size range of75–125nm forthe VGs-GS/CC samples. VGs on Cu particles within a small diameter of75–125nm like convex films, causing the area density of VGs on Cu particles decreased.Under a less screening from neighboring VGs, the emitting efficiency becomesgreatly enhanced.
(2) In the low-field region where2.1
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