E. Armour, S.Z. Sun, K. Zheng, D. P. Kopchik, C. Schaus
{"title":"AlGaAs Regrown On AiGaAs By MOCVD","authors":"E. Armour, S.Z. Sun, K. Zheng, D. P. Kopchik, C. Schaus","doi":"10.1109/LEOSST.1991.638935","DOIUrl":null,"url":null,"abstract":"Epitaxial regrowth on existing epilayers is an important technique in obtaining complicated nonplanar device geometries requiring intermediary processing steps between epitaxial growths. Such processing is an important step in the realization of optoelectronic integrated circuits (OEIC's). However, one of the major difficulties encountered with regrowth on the AlGaAs system is that the episurfaces are exposed to atmosphere during processing steps. These surfaces oxidize, forming a layer of interface states which degrade device performance. In this study, several methods have been investigated to reduce these interface states, thereby improving device characteristics. Currently, no growth technique exists to completely eliminate surface states formed at the regrowth interface. Previously, two methods have been used to reduce the effects of these states. The first method is to remove the interface region with an in-situ etchant (usually HCI) before beginning the second growth. The second method is to passivate the exposed surface using an inorganic sulfide, which ties up the oxygen bonds so that the reactivity with the aluminum species is reduced. In this study, these two methods are investigated to determine their effect on the electrical and optical characteristics of regrown laser diodes. The samples were grown in a horizontal MOCVD reactor at 100 Torr. The growths were conducted at a temperature of 725\" C, a V/III ratio of 50, and a growth rate of 500 &min. The sources used for AlGaAs were 100% arsine, trimethylgallium, and trimethylaluminum. Diethyltellurium (74 ppm in H2) was used as an n-type dopant and carbon tetrachloride (489 ppm in H2) was used as a p-type dopant in the laser structures. In the regular. single-growth structures, the (100) GaAs substrate cleaning procedure consists of successive rinses in trichloroethylene, acetone, isopropyl alcohol, and deionized water. The cleaning procedure is then followed with a light etch consisting of NQOH:H202:H20 (1:1:400) for 15 seconds. The wafers are then spun dry before being loaded into the reactor through a load-locked glove box. A hightemperature pregrowth heat treatment is usually conducted prior to the in-situ HCl etching step. The heat treatment consists of exposing the wafer to an elevated temperature of 780\" C under an arsine overpressure for 5 minutes. For the regrown samples, the same cleaning and etching procedure was used, which is subsequently followed by spinning on the ammonium sulfide solution, (\"4)2S. before loading into the reactor. The time between application of the (NH4)zS and the exposure to the oxygen-free reactor atmosphere was approximately 5 minutes. The time elapsed between the initial growth and the regrowth was approximately 24 hours, during which the AlGaAs layers were exposed to atmosphere under a laminar flow hood. Several problems with in-situ HC1 etching result from the fact that the interface region can be quite thick. A deep etch to remove the interface defects can significantly alter the non-planar structure created before the epitaxial regrowth. In addition, the depth of the etch can be hard to control and deep etches can ruin the surface morphology of the regrown layers. Hence, it is important to precisely control the etch depth to minimize these problems. To determine the etch depth for various HC1 exposure times, portions of a wafer were masked off with Si3N4 and subsequently cleaned and etched as described above. After loading the samples into the reactor, the normal growth routine of a heat treatment and HCI etch were conducted. The step between the masked and unmasked regions was then measured to give the etch depth. As shown in Fig. 1, the HC1 etch depth is a linear function in time with a constant substrate temperature and HCI flow. This relationship allows precise control of the etch depth. As expected, the GaAs etch rate is faster than AlGaAs with a decreasing etch rate as the aluminum content of the alloy is increased. Next, the concentration and thickness of the interface state layers were investigated with several test structures containing aluminum compositions of x=O.1 and x=0.4. The first growth consisted of a 3 p m AlXGal-,As layer ( n = l ~ l O ~ ~ cm9), a 2500 A AIxGal.As layer ( n = l ~ l O ~ ~ cm3), and a 50 8, undoped GaAs cap layer. Roughly 100 A of the test structure was then chemically etched with the 1:1:400 solution to expose the AI,Gal-,As oxidizing layer. After an exposure time of 24 hours, the samples were cleaned, light etched and the interface treatments were applied. The four interface treatments investigated were heat treatment only, heat treatment with (\"4)2S surface passiLation, heat treatment with a 700 A HCI etch, and heat","PeriodicalId":435740,"journal":{"name":"LEOS 1991 Summer Topical Meetings on Epitaxial Materials and In-Situ Processing for Optoelectronic Devices. Photonics and Optoelectronics","volume":"1 1","pages":"0"},"PeriodicalIF":0.0000,"publicationDate":"1900-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"LEOS 1991 Summer Topical Meetings on Epitaxial Materials and In-Situ Processing for Optoelectronic Devices. Photonics and Optoelectronics","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1109/LEOSST.1991.638935","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
Abstract
Epitaxial regrowth on existing epilayers is an important technique in obtaining complicated nonplanar device geometries requiring intermediary processing steps between epitaxial growths. Such processing is an important step in the realization of optoelectronic integrated circuits (OEIC's). However, one of the major difficulties encountered with regrowth on the AlGaAs system is that the episurfaces are exposed to atmosphere during processing steps. These surfaces oxidize, forming a layer of interface states which degrade device performance. In this study, several methods have been investigated to reduce these interface states, thereby improving device characteristics. Currently, no growth technique exists to completely eliminate surface states formed at the regrowth interface. Previously, two methods have been used to reduce the effects of these states. The first method is to remove the interface region with an in-situ etchant (usually HCI) before beginning the second growth. The second method is to passivate the exposed surface using an inorganic sulfide, which ties up the oxygen bonds so that the reactivity with the aluminum species is reduced. In this study, these two methods are investigated to determine their effect on the electrical and optical characteristics of regrown laser diodes. The samples were grown in a horizontal MOCVD reactor at 100 Torr. The growths were conducted at a temperature of 725" C, a V/III ratio of 50, and a growth rate of 500 &min. The sources used for AlGaAs were 100% arsine, trimethylgallium, and trimethylaluminum. Diethyltellurium (74 ppm in H2) was used as an n-type dopant and carbon tetrachloride (489 ppm in H2) was used as a p-type dopant in the laser structures. In the regular. single-growth structures, the (100) GaAs substrate cleaning procedure consists of successive rinses in trichloroethylene, acetone, isopropyl alcohol, and deionized water. The cleaning procedure is then followed with a light etch consisting of NQOH:H202:H20 (1:1:400) for 15 seconds. The wafers are then spun dry before being loaded into the reactor through a load-locked glove box. A hightemperature pregrowth heat treatment is usually conducted prior to the in-situ HCl etching step. The heat treatment consists of exposing the wafer to an elevated temperature of 780" C under an arsine overpressure for 5 minutes. For the regrown samples, the same cleaning and etching procedure was used, which is subsequently followed by spinning on the ammonium sulfide solution, ("4)2S. before loading into the reactor. The time between application of the (NH4)zS and the exposure to the oxygen-free reactor atmosphere was approximately 5 minutes. The time elapsed between the initial growth and the regrowth was approximately 24 hours, during which the AlGaAs layers were exposed to atmosphere under a laminar flow hood. Several problems with in-situ HC1 etching result from the fact that the interface region can be quite thick. A deep etch to remove the interface defects can significantly alter the non-planar structure created before the epitaxial regrowth. In addition, the depth of the etch can be hard to control and deep etches can ruin the surface morphology of the regrown layers. Hence, it is important to precisely control the etch depth to minimize these problems. To determine the etch depth for various HC1 exposure times, portions of a wafer were masked off with Si3N4 and subsequently cleaned and etched as described above. After loading the samples into the reactor, the normal growth routine of a heat treatment and HCI etch were conducted. The step between the masked and unmasked regions was then measured to give the etch depth. As shown in Fig. 1, the HC1 etch depth is a linear function in time with a constant substrate temperature and HCI flow. This relationship allows precise control of the etch depth. As expected, the GaAs etch rate is faster than AlGaAs with a decreasing etch rate as the aluminum content of the alloy is increased. Next, the concentration and thickness of the interface state layers were investigated with several test structures containing aluminum compositions of x=O.1 and x=0.4. The first growth consisted of a 3 p m AlXGal-,As layer ( n = l ~ l O ~ ~ cm9), a 2500 A AIxGal.As layer ( n = l ~ l O ~ ~ cm3), and a 50 8, undoped GaAs cap layer. Roughly 100 A of the test structure was then chemically etched with the 1:1:400 solution to expose the AI,Gal-,As oxidizing layer. After an exposure time of 24 hours, the samples were cleaned, light etched and the interface treatments were applied. The four interface treatments investigated were heat treatment only, heat treatment with ("4)2S surface passiLation, heat treatment with a 700 A HCI etch, and heat
在现有的外延层上进行外延再生是获得复杂的非平面器件几何形状的重要技术,需要在外延生长之间进行中间加工步骤。这种处理是实现光电集成电路(OEIC)的重要步骤。然而,在AlGaAs系统上再生遇到的主要困难之一是在处理步骤中,表面暴露在大气中。这些表面氧化,形成一层降低器件性能的界面状态。在本研究中,研究了几种方法来减少这些界面状态,从而改善器件特性。目前,还没有一种生长技术可以完全消除再生界面形成的表面态。以前,有两种方法被用来减少这些状态的影响。第一种方法是在开始第二次生长之前用原位蚀刻剂(通常是HCI)去除界面区域。第二种方法是使用无机硫化物钝化暴露的表面,无机硫化物会束缚氧键,从而降低与铝的反应性。在本研究中,研究了这两种方法对再生激光二极管电学和光学特性的影响。样品在100托的水平MOCVD反应器中生长。生长温度为725℃,V/III比为50,生长速率为500 &min。AlGaAs的来源为100%砷、三甲基镓和三甲基铝。在激光结构中,二乙基碲(74 ppm H2)作为n型掺杂剂,四氯化碳(489 ppm H2)作为p型掺杂剂。在常规的。单生长结构,(100)GaAs衬底清洗程序包括在三氯乙烯、丙酮、异丙醇和去离子水中连续冲洗。然后用NQOH:H202:H20(1:1:400)组成的光蚀刻15秒进行清洗。然后将硅片纺干,然后通过负载锁定手套箱装入反应器。在原位HCl蚀刻步骤之前,通常进行高温预生长热处理。热处理包括将晶圆片暴露在780" C的高温下,在超压下5分钟。对于再生样品,使用相同的清洗和蚀刻程序,随后在硫化铵溶液(“4”2S)上旋转。在装载到反应堆之前。施用(NH4)zS和暴露于无氧反应堆气氛之间的时间约为5分钟。初始生长和再生长之间的时间间隔约为24小时,在此期间,AlGaAs层在层流罩下暴露于大气中。原位HC1蚀刻的几个问题是由于界面区域可能相当厚。深蚀刻去除界面缺陷可以显著改变在外延再生之前产生的非平面结构。此外,蚀刻的深度很难控制,深度蚀刻会破坏再生层的表面形态。因此,精确控制蚀刻深度以尽量减少这些问题是很重要的。为了确定不同HC1曝光时间下的蚀刻深度,用Si3N4掩盖晶圆片的部分,随后如上所述进行清洗和蚀刻。将样品装入反应器后,进行热处理和HCI蚀刻的正常生长程序。然后测量遮罩和未遮罩区域之间的步长以给出蚀刻深度。如图1所示,在衬底温度和HCI流量恒定的情况下,HC1蚀刻深度是时间的线性函数。这种关系允许精确控制蚀刻深度。正如预期的那样,随着合金中铝含量的增加,GaAs的蚀刻速率比AlGaAs快,并且蚀刻速率降低。然后,用含铝成分x= 0的几种测试结构研究了界面态层的浓度和厚度。1和x=0.4。第一次生长由3 p m的AlXGal-,As层(n = 1 ~ 1 O ~ ~ cm)和2500 a的AIxGal组成。As层(n = l ~ l O ~ ~ cm3)和508,未掺杂的GaAs帽层。然后用1:1:400溶液化学蚀刻大约100 A的测试结构,以暴露AI,Gal-,As氧化层。曝光24小时后,对样品进行清洗、光蚀刻和界面处理。所研究的四种界面处理分别是单纯热处理、(4)2S表面钝化热处理、700 a HCI蚀刻热处理和加热