硅基LED量子阱相关特性及芯片p面技术研究
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摘要
硅衬底GaN基LED的研制成功,改写了以蓝宝石、碳化硅为衬底的GaN基LED的历史,是一条更具发展潜力的LED产业化技术路线,吸引了全球数十家研究单位和公司投入相关研究。在硅衬底上生长GaN材料与在蓝宝石、碳化硅衬底上生长相比,应力状态迥然不同,应力影响材料的极化,特别影响了作为有源层量子阱的生长特性和极化特性,进而影响LED的发光效率。同时,LED发展至今,在发光本质方面仍有不少重要的物理问题未搞清楚。另外,衬底不同决定了芯片端制造方面的差异化,硅材料与蓝宝石、碳化硅相比,物理、化学及加工特性方面有很大差别,通常用在蓝宝石基LED的芯片加工技术大部分不再适用于硅基LED,因此,发展一条先进的可产业化的硅基LED芯片制造技术同等重要。
本文从量子阱相关特性及芯片技术两个方面着入研究,一方面改变量子阱的生长工艺、结构设计,通过光致发光(PL)、电致发光(EL)、荧光(FL)等手段分析量子阱的发光特性。另一方面改进芯片p面接触,优化p面钝化,探索出一条电镀金属基板的硅基TF芯片技术。基于以上两个方面,本文取得了以下重要的研究结果：
1.通过研究具有单色单量子阱及单色多量子阱的硅基绿光LED的变温EL特性,发现与单色多量子阱相比,单色单量子阱LED具有更低的工作电压,小电流密度段(1～10A/cm2)具有更大的发光效率,在小电流应用方面具有更大的优势。
2.通过研究具有单色及多色量子阱的硅基绿光LED在低温下的光谱行为,发现在低温小电流密度(～10-1A/cm2)时,多量子阱LED的发光主要来自靠近n-GaN的量子阱,在低温中电流密度时(1～10A/cm2),靠近p-GaN的量子阱的发光占主要地位,在大电流密度段(～102A/cm2)时,最后一个阱的发光趋于饱和,中间量子阱的发光开始逐渐占有明显的地位。
3.建立了一个变温EL-IQE曲线与量子阱能带倾斜之间的定性关系,通过应力调制的量子阱能带倾斜模型,较好地解释了单色单量子阱和多量子阱LED在变温变电流时的众多EL特性。
4.通过研究IQE和FWHM随电流密度的变化特性,发现低温下载流子可能优先在量子阱局域态中发生复合,并在低温100K下观察到了与此相关的发光情况。
5.报道了硅基绿光LED的最高EL-IQE:工作状态下(52A/cm2),SQW-LED(@522nm)室温下的IQE为26.3%,同波长的MQW-LED为40.7%。
6.研究了量子阱个数对硅基绿光LED光学特性的影响。结果表明,4J样品的发光效率最高,2J样品的发光效率最低。荧光显微图片并非越均匀对应的发光效率越高,2J样品具有最均匀分布的荧光显微镜图片,却具有最低的发光效率。
7.采用垒掺杂的手段实现不同位置的阱发光,不同位置的垒掺硅对EL波长的影响较大。工作状态下,具有两个发光阱样品的发光效率最低,四个发光阱样品的发光效率最高。另外,垒掺杂能够使FL的均匀性明显变好,掺硅垒的位置离注入层越近,反压越低,ESD性能也越差。对比了注入层掺硅与注入层不掺硅的样品,实验现象一致反映,阱前掺硅量增加引起量子阱受到的压应力增加。
8.通过在硅衬底LED薄膜p-GaN表面蒸发不同厚度的Ni覆盖层,将其在N2：O2=4：1的气氛中、450℃-750℃的温度范围内进行退火,在去掉薄膜表面Ni覆盖层之后制备Pt/p-GaN欧姆接触层。实验结果表明：退火温度和Ni覆盖层厚度均对硅衬底GaN基LED薄膜p型欧姆接触有重要影响,Ni覆盖退火能够显著降低p型层中Mg受主的激活温度。经牺牲Ni退火后,p型比接触电阻率随退火温度的升高呈先变小后变大的规律,随Ni覆盖层厚度的增加呈先变小后变大随后又变小的趋势；经过优化后,当Ni覆盖层厚度为1.5nm,退火温度为450℃,Pt与p-GaN比接触电阻率在不需要二次退火的情况下达到6.1×10-5Ω·cm2。
9.利用硫酸双氧水选择性腐蚀经牺牲Ni退火后的LED薄膜表面。结果表明,经牺牲Ni550℃退火后,薄膜表面开始受到破坏,且随退火温度的升高,受破坏的程度增加。退火后的LED薄膜经沸腾硫酸双氧水腐蚀后,表面出现明显的腐蚀坑,我们认为这种腐蚀坑可能与材料内位错在表面的露头及由于重掺杂、量子阱内V型坑引起的p型材料的极性反转有关,且牺牲Ni退火促进了这种腐蚀坑的形成和长大。
10.讨论了金属或者绝缘材料作为p面钝化材料的可行性。通常用作n型接触的Cr,在银合金条件下完全可以达到p面钝化效果。最后讨论了是否能够选择不导电的绝缘物作为p面钝化材料,结合硅基TF芯片工艺对其进行了可行性论证：若LED芯片工艺过程不存在大应力作用,采用氮化硅、氧化硅或PI等作为p面钝化材料是可行的。
11.通过电镀的方法分别将Si衬底GaN LED薄膜转移至铜铬、铜镍基板上,并制备成不同电镀基板的LED芯片,芯片加工过程中,LED薄膜由张应力变为压应力,随后压应力不断得到释放,通过对比不同电镀金属基板LED芯片在力学、热学、光电等方面的性能可知,电镀铜镍基板LED芯片的散热性能更好、波长漂移特性更佳、力学特性以及伏安特性更加可靠。Si衬底GaN电镀金属基板LED芯片的研制成功,进一步降低了LED的制备成本。
以上研究结果已在本单位863计划相关课题研究和相关产业化过程中得到应用,取得了较好的效果。
The successful development of GaN-based LED on silicon substrate overwrites the history of InGaN LEDs only grown on sapphire and Silicon carbon, which has the more potential for industry technical route and it had attracted many relevant researches coming from dozens of research units and companies in the world. Recently, several units have reported their new research results on LEDs on Si substrate, but there has been apart from the results of LEDs on sapphire and SiC substrates, which mainly reflects in the lumen efficiency and industrialization technologies. The stress of GaN grown on Si is different from the stress of grown on sapphire and SiC, leading to the discrepancy of polarization in the materials, especially affect the properties correlated with growth and polarity, which is crucial for the lumen efficiency of LED. Up to the present, some important physical issue about the light emitting essence has not been clear. In addition, different substrate materials induce the discrepancy of chip process. The physical and chemical characters among silicon, sapphire and SiC are widely different, this result in that the chip process of LEDs on sapphire is not adapt to LEDs on Silicon. Therefore, the development of an advanced chip manufacturing technology of LED on silicon is equally important.
From the research into relevant characteristics of the quantum well and chip technology, we change the growth process and structural design of quantum well, then by photoluminescence (PL), electroluminescence (EL), fluorescence (FL) and other means, we analysis the luminescence properties of quantum wells. Otherwise, we improve p-type contact of the chip and optimize the process of p-surface passivation, explore a thin film LED chip technology by electroplating a metal substrate to replace original silicon substrate. Based on the above aspects, we find the following important results:
Through discussion of variable temperature EL features of a monochrome single quantum well and monochrome multi-quantum-well green LEDs on Si, we find that compared with the monochrome multi-quantum well, monochrome luminous efficiency. In addition, Si-doping of barrier can make FL picture uniform significantly. However, the closer of the position between the Si-doped barrier and the injection layer, the lower of the reverse voltage, the worse of ESD performance. Contrast samples of injection layer doped silicon or not, experimental results reflect consistently that the doped silicon before the well increases the compressive stress in well.
Different thick. Ni layers were deposited on the GaN-based LED films grown on Si(111) substrate, then LED films are annealed at400℃～750℃in the Atmosphere of N2:O2=4:1. The Pt/p-GaN contact layer is prepared after removing the Ni-capping layer. It is found that, annealing temperature and thickness of Ni-capping layer each have an important influence on the p-type contacts of GaN-based LED films. The Ni film can significantly reduce the activation temperature of Mg acceptor of the p-type GaN. The characteristic of p-type contact of Ni-capping sample becomes better first then turns worse with the annealing temperature and it becomes better then turns worse and then better with Ni-capping thickness. After optimization, the specific contact resistivity of Pt/p-GaN in the case of no second annealing can be reach6.1×10-5Ω·cm2, when Ni-assisted layer thickness is1.5nm and its annealing temperature is450℃.
The effects of Ni-assisted annealing on the surface morphologies of GaN-based LED films on Si substrate were studied. A wet etching method using acid-hydrogen peroxide was adopted to boil films surface after activation. We found that some nano-pits appeared on surfaces while original surface step structure was still clearly visible, which shows a defect-selective etching characteristic. Otherwise, we demonstrate the surface morphology can be affected by Ni-assisted annealing. We explain the forming reason of the pits maybe related to dislocation outcrops and polarity inversion of p-GaN which caused by heavily doped and V-pits in quantum wells. The formation and growth of corrosion pits after acid-hydrogen peroxide etched was promoted by Ni-capping annealing.
Discussing the feasibility of metal or insulating material as the material of p-surface passivation. Cr is used as the n-type contact usually, of which the purpose of p-surface passivation can be achieved under the conditions of the silver alloy. Finally, combined with silicon-based TF-chip technology, if be able to choose a non-conductive insulating material as a p-surface passivation material, and its feasibility is if the LED chip process does not exist large stress, the use of silicon nitride, silicon oxide or PI as a p-surface passivation material is feasible.
GaN LED films grown on Si (111) substrate were transfer onto copper, chromium, and copper, nickel metal substrates by electroplating separately. In chip processing, LED film is by tensile stress into compressive stress, then compressive stress continuously released. The study had found that CuNi substrate had the better heat dispersion property than CuCr substrate. The high resolution XRD show that the residual tensile stress exists in the LED film on CuCr substrate and the compressive stress exist in the LED film on CuNi substrate. CuNi LED had the stable electrical performance after aging192h under the condition of room temperature,900mA. The reliability of electroplated CuNi substrate LED had reached the demands of commercialization.
Above results have been used in the research on related National High Technology Research and Development Program863of our institute and in related industrialization. Good effects have been achieved.
本文从量子阱相关特性及芯片技术两个方面着入研究,一方面改变量子阱的生长工艺、结构设计,通过光致发光(PL)、电致发光(EL)、荧光(FL)等手段分析量子阱的发光特性。另一方面改进芯片p面接触,优化p面钝化,探索出一条电镀金属基板的硅基TF芯片技术。基于以上两个方面,本文取得了以下重要的研究结果：
1.通过研究具有单色单量子阱及单色多量子阱的硅基绿光LED的变温EL特性,发现与单色多量子阱相比,单色单量子阱LED具有更低的工作电压,小电流密度段(1～10A/cm2)具有更大的发光效率,在小电流应用方面具有更大的优势。
2.通过研究具有单色及多色量子阱的硅基绿光LED在低温下的光谱行为,发现在低温小电流密度(～10-1A/cm2)时,多量子阱LED的发光主要来自靠近n-GaN的量子阱,在低温中电流密度时(1～10A/cm2),靠近p-GaN的量子阱的发光占主要地位,在大电流密度段(～102A/cm2)时,最后一个阱的发光趋于饱和,中间量子阱的发光开始逐渐占有明显的地位。
3.建立了一个变温EL-IQE曲线与量子阱能带倾斜之间的定性关系,通过应力调制的量子阱能带倾斜模型,较好地解释了单色单量子阱和多量子阱LED在变温变电流时的众多EL特性。
4.通过研究IQE和FWHM随电流密度的变化特性,发现低温下载流子可能优先在量子阱局域态中发生复合,并在低温100K下观察到了与此相关的发光情况。
5.报道了硅基绿光LED的最高EL-IQE:工作状态下(52A/cm2),SQW-LED(@522nm)室温下的IQE为26.3%,同波长的MQW-LED为40.7%。
6.研究了量子阱个数对硅基绿光LED光学特性的影响。结果表明,4J样品的发光效率最高,2J样品的发光效率最低。荧光显微图片并非越均匀对应的发光效率越高,2J样品具有最均匀分布的荧光显微镜图片,却具有最低的发光效率。
7.采用垒掺杂的手段实现不同位置的阱发光,不同位置的垒掺硅对EL波长的影响较大。工作状态下,具有两个发光阱样品的发光效率最低,四个发光阱样品的发光效率最高。另外,垒掺杂能够使FL的均匀性明显变好,掺硅垒的位置离注入层越近,反压越低,ESD性能也越差。对比了注入层掺硅与注入层不掺硅的样品,实验现象一致反映,阱前掺硅量增加引起量子阱受到的压应力增加。
8.通过在硅衬底LED薄膜p-GaN表面蒸发不同厚度的Ni覆盖层,将其在N2：O2=4：1的气氛中、450℃-750℃的温度范围内进行退火,在去掉薄膜表面Ni覆盖层之后制备Pt/p-GaN欧姆接触层。实验结果表明：退火温度和Ni覆盖层厚度均对硅衬底GaN基LED薄膜p型欧姆接触有重要影响,Ni覆盖退火能够显著降低p型层中Mg受主的激活温度。经牺牲Ni退火后,p型比接触电阻率随退火温度的升高呈先变小后变大的规律,随Ni覆盖层厚度的增加呈先变小后变大随后又变小的趋势；经过优化后,当Ni覆盖层厚度为1.5nm,退火温度为450℃,Pt与p-GaN比接触电阻率在不需要二次退火的情况下达到6.1×10-5Ω·cm2。
9.利用硫酸双氧水选择性腐蚀经牺牲Ni退火后的LED薄膜表面。结果表明,经牺牲Ni550℃退火后,薄膜表面开始受到破坏,且随退火温度的升高,受破坏的程度增加。退火后的LED薄膜经沸腾硫酸双氧水腐蚀后,表面出现明显的腐蚀坑,我们认为这种腐蚀坑可能与材料内位错在表面的露头及由于重掺杂、量子阱内V型坑引起的p型材料的极性反转有关,且牺牲Ni退火促进了这种腐蚀坑的形成和长大。
10.讨论了金属或者绝缘材料作为p面钝化材料的可行性。通常用作n型接触的Cr,在银合金条件下完全可以达到p面钝化效果。最后讨论了是否能够选择不导电的绝缘物作为p面钝化材料,结合硅基TF芯片工艺对其进行了可行性论证：若LED芯片工艺过程不存在大应力作用,采用氮化硅、氧化硅或PI等作为p面钝化材料是可行的。
11.通过电镀的方法分别将Si衬底GaN LED薄膜转移至铜铬、铜镍基板上,并制备成不同电镀基板的LED芯片,芯片加工过程中,LED薄膜由张应力变为压应力,随后压应力不断得到释放,通过对比不同电镀金属基板LED芯片在力学、热学、光电等方面的性能可知,电镀铜镍基板LED芯片的散热性能更好、波长漂移特性更佳、力学特性以及伏安特性更加可靠。Si衬底GaN电镀金属基板LED芯片的研制成功,进一步降低了LED的制备成本。
以上研究结果已在本单位863计划相关课题研究和相关产业化过程中得到应用,取得了较好的效果。
The successful development of GaN-based LED on silicon substrate overwrites the history of InGaN LEDs only grown on sapphire and Silicon carbon, which has the more potential for industry technical route and it had attracted many relevant researches coming from dozens of research units and companies in the world. Recently, several units have reported their new research results on LEDs on Si substrate, but there has been apart from the results of LEDs on sapphire and SiC substrates, which mainly reflects in the lumen efficiency and industrialization technologies. The stress of GaN grown on Si is different from the stress of grown on sapphire and SiC, leading to the discrepancy of polarization in the materials, especially affect the properties correlated with growth and polarity, which is crucial for the lumen efficiency of LED. Up to the present, some important physical issue about the light emitting essence has not been clear. In addition, different substrate materials induce the discrepancy of chip process. The physical and chemical characters among silicon, sapphire and SiC are widely different, this result in that the chip process of LEDs on sapphire is not adapt to LEDs on Silicon. Therefore, the development of an advanced chip manufacturing technology of LED on silicon is equally important.
From the research into relevant characteristics of the quantum well and chip technology, we change the growth process and structural design of quantum well, then by photoluminescence (PL), electroluminescence (EL), fluorescence (FL) and other means, we analysis the luminescence properties of quantum wells. Otherwise, we improve p-type contact of the chip and optimize the process of p-surface passivation, explore a thin film LED chip technology by electroplating a metal substrate to replace original silicon substrate. Based on the above aspects, we find the following important results:
Through discussion of variable temperature EL features of a monochrome single quantum well and monochrome multi-quantum-well green LEDs on Si, we find that compared with the monochrome multi-quantum well, monochrome luminous efficiency. In addition, Si-doping of barrier can make FL picture uniform significantly. However, the closer of the position between the Si-doped barrier and the injection layer, the lower of the reverse voltage, the worse of ESD performance. Contrast samples of injection layer doped silicon or not, experimental results reflect consistently that the doped silicon before the well increases the compressive stress in well.
Different thick. Ni layers were deposited on the GaN-based LED films grown on Si(111) substrate, then LED films are annealed at400℃～750℃in the Atmosphere of N2:O2=4:1. The Pt/p-GaN contact layer is prepared after removing the Ni-capping layer. It is found that, annealing temperature and thickness of Ni-capping layer each have an important influence on the p-type contacts of GaN-based LED films. The Ni film can significantly reduce the activation temperature of Mg acceptor of the p-type GaN. The characteristic of p-type contact of Ni-capping sample becomes better first then turns worse with the annealing temperature and it becomes better then turns worse and then better with Ni-capping thickness. After optimization, the specific contact resistivity of Pt/p-GaN in the case of no second annealing can be reach6.1×10-5Ω·cm2, when Ni-assisted layer thickness is1.5nm and its annealing temperature is450℃.
The effects of Ni-assisted annealing on the surface morphologies of GaN-based LED films on Si substrate were studied. A wet etching method using acid-hydrogen peroxide was adopted to boil films surface after activation. We found that some nano-pits appeared on surfaces while original surface step structure was still clearly visible, which shows a defect-selective etching characteristic. Otherwise, we demonstrate the surface morphology can be affected by Ni-assisted annealing. We explain the forming reason of the pits maybe related to dislocation outcrops and polarity inversion of p-GaN which caused by heavily doped and V-pits in quantum wells. The formation and growth of corrosion pits after acid-hydrogen peroxide etched was promoted by Ni-capping annealing.
Discussing the feasibility of metal or insulating material as the material of p-surface passivation. Cr is used as the n-type contact usually, of which the purpose of p-surface passivation can be achieved under the conditions of the silver alloy. Finally, combined with silicon-based TF-chip technology, if be able to choose a non-conductive insulating material as a p-surface passivation material, and its feasibility is if the LED chip process does not exist large stress, the use of silicon nitride, silicon oxide or PI as a p-surface passivation material is feasible.
GaN LED films grown on Si (111) substrate were transfer onto copper, chromium, and copper, nickel metal substrates by electroplating separately. In chip processing, LED film is by tensile stress into compressive stress, then compressive stress continuously released. The study had found that CuNi substrate had the better heat dispersion property than CuCr substrate. The high resolution XRD show that the residual tensile stress exists in the LED film on CuCr substrate and the compressive stress exist in the LED film on CuNi substrate. CuNi LED had the stable electrical performance after aging192h under the condition of room temperature,900mA. The reliability of electroplated CuNi substrate LED had reached the demands of commercialization.
Above results have been used in the research on related National High Technology Research and Development Program863of our institute and in related industrialization. Good effects have been achieved.
引文
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