电子辅助化学气相沉积法（EACVD）制备纳米金刚石薄膜及其光电性能的研究
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摘要
本工作提出了采用正偏压,即EACVD方法,在α-SiC陶瓷和(100)Si晶片抛光衬底表面上沉积纳米金刚石薄膜。研究了气压、连续正偏压和正偏压增强成核对沉积金刚石薄膜的影响。用激光拉曼光谱,X射线衍射,场发射扫描电镜,高分辨透射电镜,原子力显微镜,Hall效应,I-V特性,光致发光光谱和椭偏光谱等方法对制备的金刚石薄膜的结构和性能以及相互间的影响机制进行了系统表征和分析。
研究表明,在1kPa气压下,随偏压电流从OA至10A逐渐增加,电子轰击显著加速了奇异面和邻位面上的成核生长。即:一,电子轰击使表面脱氢加速,表面悬挂键和碳氢基团吸附及成键增加,因而,成核率增加。晶核和晶芽表面较易出现(111)择优取向晶面。二,当在生成的台阶表面上又生成了大量晶芽及台阶时,表面将出现不同择优取向的晶面,而且,二次成核率明显上升。三,当表面悬挂键进一步增多时,氢对金刚石结构的稳定作用减弱。当在1kPa气压下,施加6A偏流增强成核时,在(100)Si晶片和α-SiC陶瓷抛光表面上,电子轰击使(111)金刚石晶面上产生较多(110)台阶,这些台阶以及台阶边伸出的悬挂键不但显著地提高了成核率,而且这些台阶边缘伸出的悬挂键方向与(100)晶面悬挂键方向一致,可以成为(100)定向生长的成核位置,在4 kPa气压下生长出(100)定向金刚石薄膜。在α-SiC陶瓷抛光表面存在许多(0001)邻晶面和台阶,有利于金刚石(111)晶面的成核生长。因而,在4 kPa气压下,施加连续偏流6A使α-SiC陶瓷衬底上薄膜呈现较强的(111)织构取向;而在(100)Si晶片上薄膜则呈现较强的(110)织构取向。在1kPa气压下,施加连续偏流8A时,表面出现了各种取向的晶芽和台阶,二次成核率有较大提高。因而,沉积的纳米金刚石膜表面粗糙度最低可达11nm(2μm×2μm),晶粒尺寸最小可达18nm。
Hall效应测试表明,施加连续正偏压使纳米金刚石薄膜呈现较强的p型半导体特性,空穴浓度达10~(14)cm~(-2),载流子迁移率为150 cm~2v~(-1)s~(-1),体电阻率为10~3Ω·cm。电子轰击形成的晶粒体内空位和位错缺陷中的悬挂键导致了纳米薄膜较强的p型半导体特性。该薄膜与低阻n型Si晶片衬底形成异质结,其I-V特性曲线具有明显的整流特性。而不施加连续正偏压制得的纳米薄膜具有较高的体电阻率,达到10~8Ω·cm。
椭偏光谱分析表明,不施加正偏压沉积制得的纳米膜折射率为2.33,低于天然金刚石折射率,消光系数接近于零。而施加连续正偏压后沉积制得的纳米膜折射率增加至2.50,大于天然金刚石折射率,消光系数也有所增加。光致发光谱分析表明,施加连续正偏压后,纳米薄膜在470 nm波长处出现较强兰色光致发光峰。而不施加正偏压沉积制得的纳米薄膜光致发光峰极其微弱。电子轰击形成的晶粒体内空位和位错缺陷中的悬挂键导致了光致发光特性。
In this work,positive bias technology,that is,electron assistance chemical vapor deposition,was applied to deposit nanocrystalline diamond films on polished surface ofα-SiC ceramics and(100)Si wafer substrates.The effects of technological parameters on the films deposition were studied.They concluded gas pressure change with positive bias,nucleation enhanced by positive bias and positive bias applied successively with deposition of the diamond films.The films structure,the films properties and their relation were characterized and analyzed by Raman spectroscopy,X-ray diffraction,field emission scanning electron microscopy,high resolution transmission electron microscopy,atomic force microscopy,Hall effective, I-V characteristic curves,photoluminescence spectroscopy and ellipsometry spectroscopy.
The results show,when positive bias was applied from 0A to 10A bias current at 1kPa gas pressure,nucleation and growth were accelerated notably by electron bombardment on singular faces and vicinal faces.That is,first,with electron bombardment H desorptions speeded up,more dangling bonds were produced and adsorption and bonding of CH groups were increased on surface,therefore, nucleation rate increase remarkably.Surfaces of embryos and nucleus often appeared (111) facet;Secondly,when another embryos and nucleus were formed again on the surfaces of steps which had been produced previously,the film surfaces appeared various orientation faces,and the secondary nucleation rates increased notably; Thirdly,when dangling bonds increased further with electron bombardment,the effect of H on stability of diamond structure was reduced.When bias current 6A was applied at 1kPa gas pressure to enhance nucleation on the polished surface of the (100) Si wafer andα-SiC ceramics,electron bombardment produced more(110) steps on the diamond(111) facets.More dangling bonds on the edge of the steps increased remarkably nucleation rate.However,the dangling bond directions agreed with the ones on(100) faces,so the steps with the dangling bonds became suitable nucleation sites which can be used to grow(100) oriented diamond films.Therefore, nucleation rate of(100) oriented growth was increased tremendously by these dangling bonds.Under the condition of 4kPa gas pressure,(100) oriented diamond film can grow on these nucleation sites.There are many(0001) vicinal faces and steps on the polished surface ofα-SiC ceramics,which aid in increasing growth rate on(111) diamond face.So,applying positive bias successively leads to stronger(111) texture of the diamond films onα-SiC ceramics substrates and stronger(110) texture of the diamond films on(100) Si wafer substrates.When bias current 8A was applied successively at 1kPa gas pressure with deposition of the films,surfaces appeared various orientation embryos and steps,and the second nucleation rate increased notably.So,the surface roughness of the nanocrystalline diamond films can reach to lowest value 11nm(scan size:2μm×2μm );the grain size can reach to smallest value 18nm.
Hall effective measurement show,when positive bias was applied successively with deposition,the nanocrystalline films deposited exhibited stronger p type semiconductor characterization,hole concentration reached to 10 ~(14) cm~(-2) carrier migration rate reached to 150cm~2v~(-1)s~(-1),bulk resistance rate reached to 10 ~3Ωcm. The dangling bonds in vacancy and dislocation,which were produced by electron bombardment,resulted in the stronger p type semiconductor characterization of the films.Heterojunction between the nanocrystalline films and low resistance n type Si wafer substrate has obvious rectification characteristic showed in I-V curve.Without applying positive bias,bulk resistance of the nanocrystalline films deposited can reach to 10 ~8Ωcm.
Ellipsometry spectroscopy measurement show,when the nanocrystalline diamond films were deposited without biasing,the films had an index of refraction of 2.33 which was lower than that of natural diamond,and coefficient of extinction was close to zero.When the nanocrystalline diamond films were deposited with positive bias applied successively,the index of refraction of the films increased to 2.50 which was higher than that of natural diamond,meanwhile the coefficient of extinction of the films increased.Photoluminescence spectroscopy measurement show,when positive bias was applied successively with deposition,the nanocrystalline diamond films exhibited a stronger blue photoluminescence peak at 470nm wave length;but the photoluminescence peak of the films deposited without applying positive bias was very weak.The dangling bonds in vacancy and dislocation,which were produced by electron bombardment,resulted in blue photoluminescence peak of the films.
研究表明,在1kPa气压下,随偏压电流从OA至10A逐渐增加,电子轰击显著加速了奇异面和邻位面上的成核生长。即:一,电子轰击使表面脱氢加速,表面悬挂键和碳氢基团吸附及成键增加,因而,成核率增加。晶核和晶芽表面较易出现(111)择优取向晶面。二,当在生成的台阶表面上又生成了大量晶芽及台阶时,表面将出现不同择优取向的晶面,而且,二次成核率明显上升。三,当表面悬挂键进一步增多时,氢对金刚石结构的稳定作用减弱。当在1kPa气压下,施加6A偏流增强成核时,在(100)Si晶片和α-SiC陶瓷抛光表面上,电子轰击使(111)金刚石晶面上产生较多(110)台阶,这些台阶以及台阶边伸出的悬挂键不但显著地提高了成核率,而且这些台阶边缘伸出的悬挂键方向与(100)晶面悬挂键方向一致,可以成为(100)定向生长的成核位置,在4 kPa气压下生长出(100)定向金刚石薄膜。在α-SiC陶瓷抛光表面存在许多(0001)邻晶面和台阶,有利于金刚石(111)晶面的成核生长。因而,在4 kPa气压下,施加连续偏流6A使α-SiC陶瓷衬底上薄膜呈现较强的(111)织构取向;而在(100)Si晶片上薄膜则呈现较强的(110)织构取向。在1kPa气压下,施加连续偏流8A时,表面出现了各种取向的晶芽和台阶,二次成核率有较大提高。因而,沉积的纳米金刚石膜表面粗糙度最低可达11nm(2μm×2μm),晶粒尺寸最小可达18nm。
Hall效应测试表明,施加连续正偏压使纳米金刚石薄膜呈现较强的p型半导体特性,空穴浓度达10~(14)cm~(-2),载流子迁移率为150 cm~2v~(-1)s~(-1),体电阻率为10~3Ω·cm。电子轰击形成的晶粒体内空位和位错缺陷中的悬挂键导致了纳米薄膜较强的p型半导体特性。该薄膜与低阻n型Si晶片衬底形成异质结,其I-V特性曲线具有明显的整流特性。而不施加连续正偏压制得的纳米薄膜具有较高的体电阻率,达到10~8Ω·cm。
椭偏光谱分析表明,不施加正偏压沉积制得的纳米膜折射率为2.33,低于天然金刚石折射率,消光系数接近于零。而施加连续正偏压后沉积制得的纳米膜折射率增加至2.50,大于天然金刚石折射率,消光系数也有所增加。光致发光谱分析表明,施加连续正偏压后,纳米薄膜在470 nm波长处出现较强兰色光致发光峰。而不施加正偏压沉积制得的纳米薄膜光致发光峰极其微弱。电子轰击形成的晶粒体内空位和位错缺陷中的悬挂键导致了光致发光特性。
In this work,positive bias technology,that is,electron assistance chemical vapor deposition,was applied to deposit nanocrystalline diamond films on polished surface ofα-SiC ceramics and(100)Si wafer substrates.The effects of technological parameters on the films deposition were studied.They concluded gas pressure change with positive bias,nucleation enhanced by positive bias and positive bias applied successively with deposition of the diamond films.The films structure,the films properties and their relation were characterized and analyzed by Raman spectroscopy,X-ray diffraction,field emission scanning electron microscopy,high resolution transmission electron microscopy,atomic force microscopy,Hall effective, I-V characteristic curves,photoluminescence spectroscopy and ellipsometry spectroscopy.
The results show,when positive bias was applied from 0A to 10A bias current at 1kPa gas pressure,nucleation and growth were accelerated notably by electron bombardment on singular faces and vicinal faces.That is,first,with electron bombardment H desorptions speeded up,more dangling bonds were produced and adsorption and bonding of CH groups were increased on surface,therefore, nucleation rate increase remarkably.Surfaces of embryos and nucleus often appeared (111) facet;Secondly,when another embryos and nucleus were formed again on the surfaces of steps which had been produced previously,the film surfaces appeared various orientation faces,and the secondary nucleation rates increased notably; Thirdly,when dangling bonds increased further with electron bombardment,the effect of H on stability of diamond structure was reduced.When bias current 6A was applied at 1kPa gas pressure to enhance nucleation on the polished surface of the (100) Si wafer andα-SiC ceramics,electron bombardment produced more(110) steps on the diamond(111) facets.More dangling bonds on the edge of the steps increased remarkably nucleation rate.However,the dangling bond directions agreed with the ones on(100) faces,so the steps with the dangling bonds became suitable nucleation sites which can be used to grow(100) oriented diamond films.Therefore, nucleation rate of(100) oriented growth was increased tremendously by these dangling bonds.Under the condition of 4kPa gas pressure,(100) oriented diamond film can grow on these nucleation sites.There are many(0001) vicinal faces and steps on the polished surface ofα-SiC ceramics,which aid in increasing growth rate on(111) diamond face.So,applying positive bias successively leads to stronger(111) texture of the diamond films onα-SiC ceramics substrates and stronger(110) texture of the diamond films on(100) Si wafer substrates.When bias current 8A was applied successively at 1kPa gas pressure with deposition of the films,surfaces appeared various orientation embryos and steps,and the second nucleation rate increased notably.So,the surface roughness of the nanocrystalline diamond films can reach to lowest value 11nm(scan size:2μm×2μm );the grain size can reach to smallest value 18nm.
Hall effective measurement show,when positive bias was applied successively with deposition,the nanocrystalline films deposited exhibited stronger p type semiconductor characterization,hole concentration reached to 10 ~(14) cm~(-2) carrier migration rate reached to 150cm~2v~(-1)s~(-1),bulk resistance rate reached to 10 ~3Ωcm. The dangling bonds in vacancy and dislocation,which were produced by electron bombardment,resulted in the stronger p type semiconductor characterization of the films.Heterojunction between the nanocrystalline films and low resistance n type Si wafer substrate has obvious rectification characteristic showed in I-V curve.Without applying positive bias,bulk resistance of the nanocrystalline films deposited can reach to 10 ~8Ωcm.
Ellipsometry spectroscopy measurement show,when the nanocrystalline diamond films were deposited without biasing,the films had an index of refraction of 2.33 which was lower than that of natural diamond,and coefficient of extinction was close to zero.When the nanocrystalline diamond films were deposited with positive bias applied successively,the index of refraction of the films increased to 2.50 which was higher than that of natural diamond,meanwhile the coefficient of extinction of the films increased.Photoluminescence spectroscopy measurement show,when positive bias was applied successively with deposition,the nanocrystalline diamond films exhibited a stronger blue photoluminescence peak at 470nm wave length;but the photoluminescence peak of the films deposited without applying positive bias was very weak.The dangling bonds in vacancy and dislocation,which were produced by electron bombardment,resulted in blue photoluminescence peak of the films.
引文
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