碳化硅薄膜的外延生长、结构表征及石墨烯的制备
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摘要
SiC作为第三代宽带隙半导体材料,具有许多优异特性,在半导体器件中有着广泛的应用。石墨烯作为一种新型的二维碳元素新材料,具有一系列优良的电学特性,例如反常的量子霍尔效应和高载流子迁移率等。这些优异性质使其成为当今研究的热点。本论文利用固源分子束外延(SSMBE)技术,在Si、Al_2O_3和SiC单晶衬底上外延生长SiC薄膜及其同质异构量子阱结构。利用MBE设备,采用高温热退火并辅助Si束流的方法,在SiC表面外延生长石墨烯。利用同步辐射以及一些常规的分析测试方法对外延生长的SiC薄膜和石墨烯进行研究。主要的研究工作及结果如下:
1 Si衬底上3C-SiC薄膜的外延生长
在Si衬底表面异质外延生长出高质量的3C-SiC薄膜,系统研究了碳化、衬底温度、Si/C束流比和预沉积Ge对Si衬底外延SiC薄膜的影响,并得到了相应的优化参数。
1)衬底Si表面的碳化调节了薄膜和衬底之间的晶格失配,缓冲了应力,从而提高了薄膜的质量。在Si表面碳化研究中,探索到了最佳的碳化温度。
2)薄膜的结晶质量在衬底温度为1000℃时最好。对于高温生长的样品,SiC薄膜和Si衬底间大的热膨胀系数失配造成界面更多的位错,导致结晶质量降低;对于低温生长的样品,衬底温度不高,原子的活性比较低,原子不能扩散到薄膜生长的能量最佳位置,因而导致低温生长的样品结晶质量下降。
3)在优化Si/C(1.5:1)比条件下生长的薄膜的质量较好。在低Si/C(1.1:1)和高的Si/C比(2.3:1)条件生长的薄膜的质量较差。可以通过控制Si/C来抑制或减少孔洞的形成,改善生长的SiC薄膜的质量
4)预沉积Ge可以提高薄膜的质量,且存在一个最佳的预沉积厚度(0.2nm)及预沉积温度。由于预沉积Ge与Si和C形成了Si_(1-x-y)Ge_xC_y合金相,它能调节晶格失配,缓冲薄膜内的应力,从而提高薄膜的质量。
2 Al_2O_3衬底上6H-SiC薄膜的外延生长
1)利用SSMBE技术,在Al_2O_3(0001)衬底上外延生长出6H-SiC薄膜。X射线Φ扫描显示出薄膜的六次对称衍射峰,表明生长的SiC薄膜接近单晶水平。
2)在优化的衬底温度下(1100℃)生长的薄膜质量较好,在较低温度(1000℃)和较高温度(1200℃)条件下生长的薄膜质量较差。
3)同步辐射掠入射X射线衍射(GID)研究表明,SiC/Al_2O_3薄膜内受到压应变,它来源于界面处SiC薄膜和蓝宝石衬底热膨胀系数的失配。薄膜远离界面后,压应变减小,单晶质量变好。GID和XRD的研究表明,薄膜内存在倾斜(tilt)和扭转(twist)畸变,且扭转大于倾斜。
3 6H-SiC表面的同质外延及量子阱结构的制备
1)预沉积Si原子后,SiC(0001)表面结构随温度的改变而变化。随着温度的升高,SiC表面的Si原子反蒸发,表面的Si原子减少并先后出现3×3和3~(1/2)×3~(1/2)重构。
2)利用不同重构表面的迁移系数的差异,调节Si束流,在衬底温度1080℃下,分别在6H-SiC(0001)的3~(1/2)×3~(1/2)和3×3重构面成功地上实现了3C-SiC和6H-SiC晶型薄膜的外延生长。
3)固定衬底温度,调节束流实现了6H-SiC/3C-SiC/6H-SiC多量子阱薄膜的外延生长,并发现该量子阱结构的宽发光带。经计算,宽发光带可能来源于不同宽度的量子阱的发光。
4 6H-SiC表面石墨烯的外延生长
1)利用超高真空MBE系统,通过高温退火并辅助Si束流的方法,在6H-SiC(0001)表面成功制备出多层石墨烯。
2)研究了不同退火时间对6H-SiC(0001)晶体外延石墨烯的影响。随着退火时间的增加,石墨烯厚度增加,样品表面孔洞减少。薄膜内存在压应力,它来源于石墨烯和SiC衬底的热膨胀系数的差异。石墨烯层数越多,应力也越小。
As a wide-band gap semiconductor material with excellent properties,SiC has many applications in the field of the semiconductor devices.Graphene,comprising of monolayer of carbon atoms packed into a two-dimensional honeycomb lattice,has a series of peculiar properties such as the anomalously quantized Hall effects,the large charge carrier mobility and so on.These peculiar properties have been promoted people to be interested in the graphene research.In this thesis,we report that the SiC films grown on different substrates of Si,SiC and Al_2O_3 and the quantum wells structure based on SiC polytype grown on 6H-SiC single crystal substrates have been produced with the method of solid source molecular beam epitaxy(SSMBE).Besides, the graphene films have also been grown on SiC surface by using the method of thermal annealing at high temperature and assisting with Si flux in the MBE chamber. Synchrotron radiation(SR) experimental technics and some normal analysis methods have been employed to investigate the grown SiC and Graphene films.The main results are listed as following.
1:The epitaxial growth of 3C-SiC films on Si substrate
The 3C-SiC films with high quality have been hetero epitaxially grown on Si substrate by the method of SSMBE.The effects of the growth factors,such as carbonization,growth temperature,Si/C flux ratio,and Ge predeposition,on the quality of SiC film have been investigated systematically and the optimized parameters have been obtained.
1) The carbonization of Si surface can accommodate the lattice mismatch,reduce the stress and improve the quality of the films.The optimized carbonized temperature is obtained on the basis of the studies above.
2) The quality of the film grown at the substrate temperature of 1000℃is the best. With higher substrate temperature,the misfit of thermal expand coefficient between SiC film and Si substrate can cause the dislocations at the interface, which affects the quality of the film.However,with lower substrate temperature, the activity of atoms is lower,thus the atoms have not enough energy to move and can not arrive the favorite positions for the growth of films,which causes the quality of the film worse.
3) The quality of the sample with the optimized Si/C flux ratio(1.5:1) is the best and the qualities of the samples with higher Si/C flux ratio(2.3:1) or lower Si/C flux ratio(1.1:1) are worse.Controlling the Si/C flux ratio can suppress the voids and improve the quality of the SiC film.
4) Ge predeposition can improve the quality of SiC film grown on Si substrate.We have optimized parameters of the amount and the temperature of Ge predeposition. The Ge predeposition induces the formation of the Si_(1-x-y)Ge_xC_y solid solution at the interface,which acts as the intermediate buffer layer to accommodate the lattice mismatch,reduce the accumulated strain of the interface and improve the quality of the SiC film.
2:The growth of 6H-SiC films on Al_2O_3 substrate
1) The 6H-SiC films have been hetero epitaxially grown on Al_2O_3(0001) substrate by the method of SSMBE.X-rayΦscan shows the six-fold symmetry of SiC(100) planes,which indicates that the grown SiC thin film is almost the single crystal film.
2) The quality of the film grown at substrate temperature of 1100℃is the best and that of the films grown at substrate temperature of 1000℃and 1200℃are worse.
3) The results of GID show that the films are under compressive stress caused by the misfit of the thermal expand coefficient between SiC film and Al_2O_3 substrate. When the internal part of the film is further away from the interface of SiC film and Al_2O_3 substrate,the strain of the SiC film decreases and the crystalline quality of the SiC film becomes better.The results of XRD and GID show that the film has different tilt mosaic and twist mosaic and the angle distribution of former is smaller than that of the latter.
3:Homoepitaxy growth of SiC film and the fabrication of SiC polytype quantum wells on 6H-SiC(0001) substrate
1) After Si predeposition,the surface structure of 6H-SiC(0001) changes with the variation of substrate temperature.When the temperature increases,the evaporation of Si atom from the surface causes the Si atoms on the surface gradually decreases.Thus 3×3 and 3~(1/2)×3~(1/2) reconstruction can be obtained.
(2) Due to the difference of diffusion coefficient of Si atoms on the different reconstruction surfaces,the 3C-SiC and 6H-SiC films have been successfully grown on 3×3 and 3~(1/2)×3~(1/2) reconstruction surfaces of 6H-SiC(0001) substrate respectively by controlling the Si flux at substrate temperature of 1080℃.
(3) The 6H-SiC/3C-SiC/6H-SiC film with quantum wells structure has been fabricated on the 6H-SiC substrate by controlling the flux at the substrate temperature of 1080℃.The intense emissions are found in a wide range of spectrum,which is attributed to the luminescence of the 6H-SiC/3C-SiC/6H-SiC quantum wells.The calculated results show that the wide range of luminescence is probably caused by the quantum wells with different width.
4:The growth of graphene on SiC surface
1) The epitaxial graphene(EG) layer has been successfully grown on Si-terminated 6H-SiC(0001) substrate by the method of thermal annealing at high temperature and assisting with Si flux in ultrahigh vacuum(UHV) molecular beam epitaxy(MBE) chamber.
2) The effect of annealing time on the growth of graphene on 6H-SiC(0001) surface is investigated.With the increase of annealing time,the thickness of graphene layer increases and the voids on the grown graphene surface decreases.There is compressive strain in the film,which is induced by the large difference between the coefficients of thermal expansion of graphene and SiC.The strain of the film becomes smaller with the increase of the layer thickness.
1 Si衬底上3C-SiC薄膜的外延生长
在Si衬底表面异质外延生长出高质量的3C-SiC薄膜,系统研究了碳化、衬底温度、Si/C束流比和预沉积Ge对Si衬底外延SiC薄膜的影响,并得到了相应的优化参数。
1)衬底Si表面的碳化调节了薄膜和衬底之间的晶格失配,缓冲了应力,从而提高了薄膜的质量。在Si表面碳化研究中,探索到了最佳的碳化温度。
2)薄膜的结晶质量在衬底温度为1000℃时最好。对于高温生长的样品,SiC薄膜和Si衬底间大的热膨胀系数失配造成界面更多的位错,导致结晶质量降低;对于低温生长的样品,衬底温度不高,原子的活性比较低,原子不能扩散到薄膜生长的能量最佳位置,因而导致低温生长的样品结晶质量下降。
3)在优化Si/C(1.5:1)比条件下生长的薄膜的质量较好。在低Si/C(1.1:1)和高的Si/C比(2.3:1)条件生长的薄膜的质量较差。可以通过控制Si/C来抑制或减少孔洞的形成,改善生长的SiC薄膜的质量
4)预沉积Ge可以提高薄膜的质量,且存在一个最佳的预沉积厚度(0.2nm)及预沉积温度。由于预沉积Ge与Si和C形成了Si_(1-x-y)Ge_xC_y合金相,它能调节晶格失配,缓冲薄膜内的应力,从而提高薄膜的质量。
2 Al_2O_3衬底上6H-SiC薄膜的外延生长
1)利用SSMBE技术,在Al_2O_3(0001)衬底上外延生长出6H-SiC薄膜。X射线Φ扫描显示出薄膜的六次对称衍射峰,表明生长的SiC薄膜接近单晶水平。
2)在优化的衬底温度下(1100℃)生长的薄膜质量较好,在较低温度(1000℃)和较高温度(1200℃)条件下生长的薄膜质量较差。
3)同步辐射掠入射X射线衍射(GID)研究表明,SiC/Al_2O_3薄膜内受到压应变,它来源于界面处SiC薄膜和蓝宝石衬底热膨胀系数的失配。薄膜远离界面后,压应变减小,单晶质量变好。GID和XRD的研究表明,薄膜内存在倾斜(tilt)和扭转(twist)畸变,且扭转大于倾斜。
3 6H-SiC表面的同质外延及量子阱结构的制备
1)预沉积Si原子后,SiC(0001)表面结构随温度的改变而变化。随着温度的升高,SiC表面的Si原子反蒸发,表面的Si原子减少并先后出现3×3和3~(1/2)×3~(1/2)重构。
2)利用不同重构表面的迁移系数的差异,调节Si束流,在衬底温度1080℃下,分别在6H-SiC(0001)的3~(1/2)×3~(1/2)和3×3重构面成功地上实现了3C-SiC和6H-SiC晶型薄膜的外延生长。
3)固定衬底温度,调节束流实现了6H-SiC/3C-SiC/6H-SiC多量子阱薄膜的外延生长,并发现该量子阱结构的宽发光带。经计算,宽发光带可能来源于不同宽度的量子阱的发光。
4 6H-SiC表面石墨烯的外延生长
1)利用超高真空MBE系统,通过高温退火并辅助Si束流的方法,在6H-SiC(0001)表面成功制备出多层石墨烯。
2)研究了不同退火时间对6H-SiC(0001)晶体外延石墨烯的影响。随着退火时间的增加,石墨烯厚度增加,样品表面孔洞减少。薄膜内存在压应力,它来源于石墨烯和SiC衬底的热膨胀系数的差异。石墨烯层数越多,应力也越小。
As a wide-band gap semiconductor material with excellent properties,SiC has many applications in the field of the semiconductor devices.Graphene,comprising of monolayer of carbon atoms packed into a two-dimensional honeycomb lattice,has a series of peculiar properties such as the anomalously quantized Hall effects,the large charge carrier mobility and so on.These peculiar properties have been promoted people to be interested in the graphene research.In this thesis,we report that the SiC films grown on different substrates of Si,SiC and Al_2O_3 and the quantum wells structure based on SiC polytype grown on 6H-SiC single crystal substrates have been produced with the method of solid source molecular beam epitaxy(SSMBE).Besides, the graphene films have also been grown on SiC surface by using the method of thermal annealing at high temperature and assisting with Si flux in the MBE chamber. Synchrotron radiation(SR) experimental technics and some normal analysis methods have been employed to investigate the grown SiC and Graphene films.The main results are listed as following.
1:The epitaxial growth of 3C-SiC films on Si substrate
The 3C-SiC films with high quality have been hetero epitaxially grown on Si substrate by the method of SSMBE.The effects of the growth factors,such as carbonization,growth temperature,Si/C flux ratio,and Ge predeposition,on the quality of SiC film have been investigated systematically and the optimized parameters have been obtained.
1) The carbonization of Si surface can accommodate the lattice mismatch,reduce the stress and improve the quality of the films.The optimized carbonized temperature is obtained on the basis of the studies above.
2) The quality of the film grown at the substrate temperature of 1000℃is the best. With higher substrate temperature,the misfit of thermal expand coefficient between SiC film and Si substrate can cause the dislocations at the interface, which affects the quality of the film.However,with lower substrate temperature, the activity of atoms is lower,thus the atoms have not enough energy to move and can not arrive the favorite positions for the growth of films,which causes the quality of the film worse.
3) The quality of the sample with the optimized Si/C flux ratio(1.5:1) is the best and the qualities of the samples with higher Si/C flux ratio(2.3:1) or lower Si/C flux ratio(1.1:1) are worse.Controlling the Si/C flux ratio can suppress the voids and improve the quality of the SiC film.
4) Ge predeposition can improve the quality of SiC film grown on Si substrate.We have optimized parameters of the amount and the temperature of Ge predeposition. The Ge predeposition induces the formation of the Si_(1-x-y)Ge_xC_y solid solution at the interface,which acts as the intermediate buffer layer to accommodate the lattice mismatch,reduce the accumulated strain of the interface and improve the quality of the SiC film.
2:The growth of 6H-SiC films on Al_2O_3 substrate
1) The 6H-SiC films have been hetero epitaxially grown on Al_2O_3(0001) substrate by the method of SSMBE.X-rayΦscan shows the six-fold symmetry of SiC(100) planes,which indicates that the grown SiC thin film is almost the single crystal film.
2) The quality of the film grown at substrate temperature of 1100℃is the best and that of the films grown at substrate temperature of 1000℃and 1200℃are worse.
3) The results of GID show that the films are under compressive stress caused by the misfit of the thermal expand coefficient between SiC film and Al_2O_3 substrate. When the internal part of the film is further away from the interface of SiC film and Al_2O_3 substrate,the strain of the SiC film decreases and the crystalline quality of the SiC film becomes better.The results of XRD and GID show that the film has different tilt mosaic and twist mosaic and the angle distribution of former is smaller than that of the latter.
3:Homoepitaxy growth of SiC film and the fabrication of SiC polytype quantum wells on 6H-SiC(0001) substrate
1) After Si predeposition,the surface structure of 6H-SiC(0001) changes with the variation of substrate temperature.When the temperature increases,the evaporation of Si atom from the surface causes the Si atoms on the surface gradually decreases.Thus 3×3 and 3~(1/2)×3~(1/2) reconstruction can be obtained.
(2) Due to the difference of diffusion coefficient of Si atoms on the different reconstruction surfaces,the 3C-SiC and 6H-SiC films have been successfully grown on 3×3 and 3~(1/2)×3~(1/2) reconstruction surfaces of 6H-SiC(0001) substrate respectively by controlling the Si flux at substrate temperature of 1080℃.
(3) The 6H-SiC/3C-SiC/6H-SiC film with quantum wells structure has been fabricated on the 6H-SiC substrate by controlling the flux at the substrate temperature of 1080℃.The intense emissions are found in a wide range of spectrum,which is attributed to the luminescence of the 6H-SiC/3C-SiC/6H-SiC quantum wells.The calculated results show that the wide range of luminescence is probably caused by the quantum wells with different width.
4:The growth of graphene on SiC surface
1) The epitaxial graphene(EG) layer has been successfully grown on Si-terminated 6H-SiC(0001) substrate by the method of thermal annealing at high temperature and assisting with Si flux in ultrahigh vacuum(UHV) molecular beam epitaxy(MBE) chamber.
2) The effect of annealing time on the growth of graphene on 6H-SiC(0001) surface is investigated.With the increase of annealing time,the thickness of graphene layer increases and the voids on the grown graphene surface decreases.There is compressive strain in the film,which is induced by the large difference between the coefficients of thermal expansion of graphene and SiC.The strain of the film becomes smaller with the increase of the layer thickness.
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