CN105821435A - 用于GaN装置的基于导电性的选择性蚀刻和其应用 - Google Patents

用于GaN装置的基于导电性的选择性蚀刻和其应用 Download PDF

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CN105821435A
CN105821435A CN201610206389.4A CN201610206389A CN105821435A CN 105821435 A CN105821435 A CN 105821435A CN 201610206389 A CN201610206389 A CN 201610206389A CN 105821435 A CN105821435 A CN 105821435A
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npgan
layer
porosity
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CN105821435B (zh
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荣格·韩
孙乾
张宇
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Yale University
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Abstract

本申请涉及用于GaN装置的基于导电性的选择性蚀刻和其应用。本发明涉及在大面积(>1cm2)上以受控孔直径、孔密度和孔隙率生成NP氮化镓(GaN)的方法。本发明还揭示基于多孔GaN生成新颖光电子装置的方法。另外揭示一种用以分离并产生独立式结晶GaN薄层的层转移方案，所述方案使得涉及衬底再循环的新装置制造模式成为可能。本发明揭示的其它实施例涉及基于GaN的纳米晶体的制造和NP GaN电极在电解、水分解或光合过程应用中的使用。

Description

用于GaN装置的基于导电性的选择性蚀刻和其应用
本申请是申请日为2011年1月27日，申请号为201180007613.2、发明名称为“用于GaN装置的基于导电性的选择性蚀刻和其应用”的发明专利申请的分案申请。
关于联邦资助研究与发展的声明
在本发明的开发期间所执行的工作的一部分是根据由美国能源部(U.S.DepartmentofEnergy)授予的许可号DE-FC26-07NT43227、DE-FG0207ER46387和DE-SC0001134利用美国政府基金(U.S.Governmentfunds)实施。美国政府对本发明拥有某些权利。
技术领域
本发明涉及处理基于GaN的半导体材料和由其形成装置的领域。
背景技术
在半导体处理领域，已对多孔硅材料关于其有益的光学和机械性质的发展给予相当多的关注。多孔硅通常是使用湿式电化学蚀刻工艺生成。
另一种特别感兴趣的材料是GaN。GaN装置在显示器、数据存储和照明应用中的重要性已经明确地建立。在过去二十年，已经在深度探索GaN的外延生长，但仍在寻找灵活的湿式蚀刻程序。
发明内容
本发明涉及用于生成纳米多孔NPGaN的方法。本发明的一种方法包含：将GaN暴露于电解液，将GaN耦合到电源的一个端子并将浸于电解液中的电极耦合到电源的另一个端子，以由此形成电路；并激励电路以增加GaN的至少一部分的孔隙率。因此，产生可用于许多基于半导体的电子和光学应用中的具有可调谐光学和机械性质的材料。还提供多种方法来控制GaN的孔隙率以生成有用的光学结构，例如具有增强的光提取性质的分布式布拉格反射器(distributedBraggreflector)、法布里-珀珞滤光片(Fabry-Perotopticalfilter)和发光二极管。还提供使用NPGaN衬底的装置制造方法和用于将NPGaN层和装置分离的方法。最后，提供用于从NPGaN生成纳米晶体的方法和用于生成NPGaN电极用于电解、水分解或光合过程应用的方法。
下文参照随附图式详细阐述其它特征和优点以及各个实施例的结构和操作。应注意，本发明并不限于本文所阐述的特定实施例。所述实施例仅出于说明性的目的而呈现于本文中。额外实施例对于所属领域的技术人员基于本文所包含的教示将显而易见。
附图说明
随附图式并入本发明中且形成说明书的一部分，其图解说明本发明且与说明书一起进一步用以解释本发明的原理并使得所属领域的技术人员能够制造和使用本发明。
图1是根据本发明的实施例GaN电化学(EC)蚀刻工艺的图解说明。
图2是根据本发明的实施例所观察到的EC工艺的相图的图解说明。
图3a到图3d图解说明根据本发明的实施例从EC工艺所产生的NPGaN的SEM显微照片。
图4a和图4b图解说明根据本发明的实施例在EC工艺期间反复地从低电压切换到高电压所产生的多层NPGaN结构。
图5a和图5b图解说明根据本发明的实施例从EC工艺中所用的多层掺杂轮廓产生的另一多层NPGaN结构。
图6a和图6b图解说明根据本发明的实施例从EC工艺产生的更复杂的多层NPGaN结构。
图7图解说明根据本发明的实施例在NPGaN上再生长GaN的工艺。
图8a到图8c图解说明根据本发明的实施例具有包埋NPGaN层的LED装置的增强的光提取的原理。
图9a到图9c图解说明根据本发明的实施例制造的具有包埋NPGaN层的LED装置结构。
图10a到图10h图解说明根据本发明的实施例用于将NPGaN连续结晶层与体衬底分离的两种方法。
图11a到图11c图解说明根据本发明的实施例在电解液中连续结晶层与体衬底的完全分离。
图12a到图12d图解说明平面SEM图像：(a)在NPGaN隔膜从衬底断裂处，(b)NPGaN隔膜的表面，(c)所暴露下伏GaN的表面，和(d)从独立式GaN隔膜的边缘的斜视图。这些材料是根据本发明的实施例生成。
图13是根据本发明的实施例制造垂直薄膜装置和再循环/回收GaN和其它衬底的途径的示意图。
图14a到图14e图解说明根据本发明的实施例用于制作GaN纳米晶体的第一种工艺。
图15a到图15c图解说明根据本发明的实施例：(a)个别GaN纳米晶体的高分辨率TEM图像，(b)来自GaN纳米晶体聚集的GaN微粒，和(c)GaN纳米晶体的光致发光和吸光度测量。
图16a和图16b图解说明根据本发明的实施例用于制作包括NP隔膜的GaN纳米晶体的第二种工艺。
图17a到图17c显示根据本发明的实施例：(a)独立式GaN隔膜/膜在溶液中的图片，其包括一个较大的薄片(由上部的两个箭头指出)和若干较小的小片和碎片(底部箭头)，(b)超声波处理1小时之后，和(c)胶状GaN纳米晶体在UV光下的发光照片。
图18是根据本发明的实施例使用NPGaN电极的水分解试验中所用的设备的图解说明。
图19图解说明根据本发明的实施例NPGaN电极在水分解试验中的有益用途，其导致降低的饱和电流密度。
具体实施方式
生成多孔GaN的方法
本发明提供在大面积(例如，大于1平方厘米)上生成具有受控孔直径、孔密度和孔隙率的纳米多孔(NP)氮化镓(GaN)的方法。另外，这些方法同样可适用于在较小的面积上生成NPGaN。
尽管整个说明书中着重于GaN，但这些技术也可应用于其它III-氮化物系统(例如InGaN)。因此，术语“GaN”在整个说明书中应广泛地解释为是指任何III-氮化物材料，例如InGaN、AlGaN等。因此，短语“NPGaN”也可解释为“NPInGaN”等。
纳米多孔GaN用于再生长、微加工、化学传感和其它应用(例如半导体电子和光学装置制造)中具有极大的潜力。其还具有用于如本文所述纳米技术应用中的适用性。本文所揭示的方法可用于直接产生平面GaN晶片，而不需要UV-激光、反应性离子蚀刻或诸如此类。所揭示的方法是有效的且与现有半导体制造技术相容。
纳米多孔GaN被视为III-氮化物化合物家族的新成员。尽管其具有极大增加的表面积，但其具有高结晶度和光电子质量。其几个重要的物理性质归纳如下：(1)NPGaN导电，其中所测量导电率与n型GaN相当(电注入装置的一种重要属性)，(2)光学折射率可利用孔隙率进行调谐以用于光学限制和改造，(3)弹性柔度(或刚度)可得到极大改进(类似海绵的行为)，而同时维持其单晶特性，和(4)可用同质外延方式实施NPGaN上的过度生长或再生长，其中可用小于10nm的GaN生长将NP表面'密封'成原子平滑度，同时仍可保留NP特性。
根据本发明的实施例，可通过利用电解液进行电化学(EC)蚀刻选择性地移除重度掺杂(即，1017cm-3到1019cm-3)的GaN。水平和垂直蚀刻两种工艺是可能的。水平蚀刻是从在未经掺杂的GaN顶层下面外延生长n型掺杂GaN层开始。接着采用干式蚀刻或解离以暴露双层或多层结构的侧壁。接着进行电化学蚀刻以水平并选择性地通过n型GaN下伏层，以实现底切。本发明阐述从表面垂直蚀刻平面n型GaN的方法，其中蚀刻在大体上垂直于晶片表面的方向上传播。这些方法详细揭示于下文中。
根据本发明实施例的EC蚀刻工艺示意性地图解说明于图1中。在实施例中，在室温下使用草酸作为电解液104。在其它实施例中，可使用其它电解液，例如KOH或HCL。n型掺杂GaN试样102和铂丝108构成阳极和阴极，其分别连接到电源106以形成电路。电源106用于激励电路，此电路驱动电流通过材料，此修改其物理性质并在材料中生成孔隙率轮廓。在各种实施例中，可通过使用测量装置(如110和112所显示)记录电流和电压并使用参考电极114(例如，由Ag/AgCl制成)来监控参考电极与阳极电极之间的电位差，来控制电流或电压。如在以下章节中所讨论，通常采用在5V到60V范围内的电压和在1018cm-3到1019cm-3范围内的n型GaN掺杂。
可采用各种时间依赖性激励技术，其中电压或电流可以脉冲方式、斜坡上升方式或类似方式输送。在此方法的实施例中，EC蚀刻之后，可将试样相继在去离子水、甲醇和戊烷中洗涤以在最后干燥工艺中使表面张力最小化，此确保任何残留蚀刻化学品的完全溶解。
通过n型掺杂的程度和所施加电压来控制EC蚀刻工艺。所观察到的蚀刻形态与所施加电压(5V到30V)和n型GaN掺杂(1018cm-3到1019cm-3)有关。草酸的浓度可在0.03M与0.3M之间变化，且未观察到强依赖性。EC蚀刻的“相图”显示于图2中。基于扫描电子显微镜(SEM)成像鉴别三个区，其包括未蚀刻202(区I)、NPGa的形成204(II)和完全层移除或电抛光206(III，包括高于30V的电压)，且电导率或所施加电压增加。在若干实施例中，举例来说，可在10V、15V和20V下在掺杂浓度在1017cm-3到1019cm-3范围内的n型GaN上执行EC蚀刻。
由上文所阐述方法产生的NPGaN形态图解说明于图3a到图3c中。图3a到图3c显示分别在10V(302)、15V(304)和20V(306)下制备的NPGaN的平面SEM图像。图3d是在15V下所制备的所得NP膜308的横截面SEM图像。
使用上文所阐述的电化学工艺，能够垂直地纳米钻孔穿过GaN层并产生具有不同孔径和孔隙率的GaN层，其相当于具有不同折射率的层。在若干实施例中，可通过改变所施加电压、电流或GaN掺杂轮廓产生GaN多层结构。具有所设计折射率轮廓的分层结构(包括四分之一波长分布式布拉格反射器(DBR))具有用于光学或生物医学应用的许多用途。
现在将阐述其中可生成有用的光电子结构和装置的实施例。基于GaN的光-电子装置可用于解决固态发光、显示器和电力电子器件中的若干问题。基于GaN的垂直腔表面发射激光(VCSEL)和共振腔发光二极管(RCLED)是所述装置的实例。这些装置的一个重要操作要求是需要通常呈分布式布拉格反射器(DBR)形式的高反射镜。VCSEL在有源区的两侧上需要高度反射的DBR镜以形成激光腔，同时对于RCLED，在有源区下面的高反射DBR可提高输出功率和发射光谱。DBR结构对于GaNVCSEL在两个方面特别重要。第一，随着DBR峰值反射率从90％增加到99％，GaNVCSEL的阈电流密度可减小一个数量级。第二，DBR将具有大的阻带带宽。这一点很重要，因为基于GaN的VCSEL的有源区通常由InGaN多重量子阱(MQW)构成，且InGaNMQW的发射峰值往往随生长条件或工艺参数的小的变化而波动。具有宽阻带的DBR可提供发射波长中所述光谱变化的足够覆盖。
揭示涉及形成NPGaN多层结构的方法的实施例。图4图解说明利用孔隙率对阳极氧化参数(例如所施加电压或电流密度402)的依赖性的实施例。例如，如图4a中所显示，通过在阳极氧化处理期间在高406或低402电压或电流密度之间切换，可获得具有高和低孔隙率(分别地，低和高折射率)的层，如图4b的408中所显示。图4b图解说明通过在阳极氧化处理期间在高和低电压或电流密度之间切换所获得的多层NPGaN的横截面SEM图像。特征410和414图解说明所得多层结构的高孔隙率，而特征412和416图解说明低孔隙率。
图5图解说明利用孔形态和孔隙率二者对个别层的电导率的依赖性的另一实施例，个别层的电导率进而可通过外延生长期间的掺杂浓度控制，如图5a中所显示。可通过掺杂源材料以具有高506和低504掺杂区来获得高512和低510孔隙率NPGaN层，其分别显示于图5b中。在此情形中，可使用恒定电压或电流蚀刻获得适宜孔隙率轮廓。
对于图4和图5中图解说明的实施例来说，所得有效介电函数具有深度依赖性，因为NPGaN层内仍保留不同的孔隙率和GaN纳米晶体尺寸二者。前述实施例具有不需要外延生长以实现具有不同掺杂剂浓度的层的优点，但低与高孔隙率GaN层之间的界面有时较粗糙。后面的实施例具有精确控制厚度和界面骤降度的优点。
在另一实施例中，使用脉冲蚀刻方法以对于极低折射率实现极高孔隙率，如图6a和图6b中所图解说明。此脉冲蚀刻不同于如图4和图5的实施例中所采用的折射率在光波长量级下的调制。图6中所图解说明的脉冲蚀刻包含高电压606与低电压604(或零电压)之间的交替。接着以重复循环进行蚀刻。使用脉冲蚀刻技术以实现极高孔隙率区612，如图6b中的SEM显微照片中所显示，而在脉冲蚀刻之前使用恒定低电压蚀刻产生低孔隙率层610，图6a中未显示。
在确定了NPGaN中孔隙率的控制之后，可以想象具有可调谐折射率的新型单晶NPGaN层。所述材料的实例显示于图6b的特征608中。举例来说，特征608图解说明在蓝宝石上的四片小片NPGaN外延层。折射率的变化改变光学腔长度，此使得在各试样之间法布里-珀珞干涉峰位移。在白色光照明下，这些材料出现彩虹色，其展示包括(例如)紫色、绿色、橙色和粉色的一系列色彩。
具有约30％孔隙率的NPGaN层可产生与AlN层同等的折射率对比，而在410-nm激光二极管中通常采用的AlGaN包覆层(Al-15％，厚度-0.5微米)可由具有约5％孔隙率的NPGaN层代替用于高效波导。
这些实施例提供一种简单灵活的途径来制造用于光学和生物医学应用的大规模NPGaN多层。其优点和用途包括：(1)具有增加的折射率对比的基于GaN的DBR对，(2)基于GaN低成本的VCSEL和RCLED，(3)法布里-珀珞滤光片，(4)用于能量转换的抗反射涂层，(5)光学生物传感器，和(6)用于III-氮化物材料和所生长装置的衬底。
用于装置应用的纳米多孔衬底
涉及使用NP衬底的方法的其它实施例包括用以以下各项的技术：(1)在蓝宝石(或III-氮化物、SiC、Si、ZnO、LiNbO3、LiAlO2等)衬底上通过电化学蚀刻制作极性、非极性和半极性NPIII-氮化物结构，(2)在NP结构上生长高质量极性、非极性和半极性III-氮化物材料，(3)使用再生长的III-氮化物材料制造极性、非极性和半极性III-氮化物光电子装置(LED、激光等)和电子装置(例如高电子迁移率晶体管(HEMT))，和(4)在NPIII-氮化物结构上通过HVPE使用再生长的III-氮化物材料产生极性、非极性和半极性III-氮化物体衬底。
图7图解说明工艺流程以及获得适用于装置制造的NPGaN模板的实施例的实验结果。在此实施例中，以使用标准外延技术生长的半极性(1122)GaN表面开始。此一表面显示于特征702中。尽管具有高缺陷密度(位错-3×109cm-2；堆栈错误-105cm-1)，但此一表面适用于制造(例如)绿色发光LED。然而，可通过应用EC蚀刻技术的实施例以产生NPGaN表面(如平面图中特征704中所显示)来生成缺陷密度极大地减小的衬底。此表面的截面图像显示于图7的右下部分中。此图像图解说明多层结构，其包含在非多孔GaN708层的顶部上的NPGaN层706，非多孔GaN708层生长在蓝宝石衬底710上。
图解说明于图7的右上和右下部分的NPGaN表面提供高质量衬底，在其上生长具有减小的缺陷密度的GaN。在NPGaN模板(衬底)上生长高质量GaN的工艺称为“再生长”且此一在生长工艺的结果图解说明于图7的左下部分中，在其中(1122)已再生长半极性GaN。EC成孔工艺并不敏感地依赖于晶体学取向。图7中所阐述的工艺已在极性、非极性和半极性GaN层上重复，其包括成孔和再生长。
光子学应用
图8图解说明先前所揭示实施例用于制造InGaN/GaN有源结构的应用，所述有源结构由于存在包埋NPGaN层(图8c中的828)而具有增强的光提取性质。此一结构是通过在NPGaN模板上生长InGaN/GaN有源结构来形成，所述NPGaN模板如先前章节中所讨论制造且图解说明于图7中。图8c图解说明具有包埋NPGaN层828的InGaN/GaN有源区，而图8b图解说明较传统的InGaN/GaN有源区结构。
图8c图解说明蓝宝石衬底826，其上已生长未掺杂GaN层824和NPGaN层828。然后在NP层上生长另一未掺杂GaN层822，随后在所述另一未掺杂GaN层上生长多重量子阱(MQW)结构820。包埋NPGaN层828的存在增加装置818中的光散射，此导致增强的光提取。
图8b图解说明以传统方式生长的没有包埋NP层的InGaN/GaN有源结构。在此结构中，未掺杂GaN层814生长于蓝宝石衬底816上，然后是使用标准技术生长的MQWLED结构812。没有包埋NP层，光在810内经历多重全内反射和再吸收，此导致低效率的光提取。
图8a呈现光致发光(PL)随距激光光斑的横向距离而变的曲线。三条曲线804、806和808对应于根据上文所揭示实施例制造的装置，其包含：无多孔层，分别具有40nm孔径和70nm孔径的多孔层。此图图解说明，具有70nm孔的装置与另外两个装置相比，在具有包埋NP层的情况下光提取效率较大。
图9更详细的图解说明在NPGaN模板906上生长的LED的装置结构。右侧的图9b和9c显示在NP层上生长的LED的截面SEM和在LED层下面的经转换空隙932的近视图。特征920涵盖图9a中的示意性装置的装置层908到912，而左边的未掺杂层908在右边的显微照片中可视为特征930。左边的NP层904和906视为右边的空隙层932，而在左边由902指示的未掺杂GaN在显微照片中视为特征934。
连续结晶层的分离
图10图解说明本发明用于生成独立式GaN隔膜和层的其它实施例。一个实施例是基于均匀掺杂的GaN层1018，且利用EC蚀刻在低电压条件(图10a中的特征1004)下进行，此导致生成具有低密度(小于109cm-2)和小直径(约30nm)的纳米孔1020和1024并垂直向下传播。一旦实现所要的厚度(对应于最终隔膜的厚度)，就增加蚀刻电压(从图10a中的1004)，此对应于相图上蚀刻条件的横向移动(到图10a中的点1008)。此条件引起GaN的快速分枝并横向蚀刻进入低孔隙率层1024下面的高孔隙率层1026。连续结晶层1030的形成和分开示意性地图解说明于图10b到10e中。
对应于图10的实施例的实验结果图解说明于图11中。第一和第二电压条件分别设定为10V和15V。第一步骤期间的蚀刻速率为200nm/min；五分钟的蚀刻足以产生厚度约1微米的低孔隙率层。当将电压增加到15V时，电化学作用加速，且在GaN表面(阳极)和铂反电极二者处观察到生成气泡。在1分钟内实现GaN薄层与试样边缘的分开，如图11中的特征1104、1108和1112所显示。在15V下继续EC蚀刻导致整个层以大的宏观面积1108漂浮。在此情形下，已分开的薄层的尺寸为约1cm2，其受试样尺寸的限制，如由图11中的特征1104、1108、1112和1116所图解说明。将溶液中的独立式GaN薄膜从溶液中取出并转移到盖玻片1116(图10b)。可以设想此程序可延伸到较大的晶片(例如，2英寸或更大)。
图12中的SEM图像显示从NPGaN隔膜的表面所观察到的孔隙率(1204和1206)差异。图12a和12b中的水平箭头显示经分开隔膜具有比剩余表面1204微细NP形态1206。图12d显示独立式NP隔膜的边缘的倾斜SEM视图，其表明隔膜的NP特性得到很好的保留且分离过程局限于GaN衬底1216上蚀刻正面1214附近。
或者，在其它实施例中，具有经改造掺杂轮廓的GaN薄层有利于更简单的EC蚀刻程序。此过程图解说明于图10f到图10h中。在此实施例(程序B)中，在重度掺杂层1036上生长具有轻度掺杂层1034的两层GaN结构。利用此一经改造轮廓，EC蚀刻工艺仅需要恒定电压。在所述条件下，NP蚀刻自发地从图10a中的1014进行到1008，其垂直横穿相图而产生类似效应。已观察到极相似的结果(即，层1038和1044的分开)，如那些图解说明于图11和12中者。鉴于现代外延技术的进步，使用包埋掺杂轮廓获得更好的控制和灵活性。
以上所揭示实施例可提供用于装置制造的GaN外延层的简单大面积转移，其可明显降低成本，同时增强其功能性。唯一的竞争技术是激光剥离(LLO)，激光剥离昂贵、耗时、不能扩大，且具有不确定的良率。
所揭示实施例的应用包括将硅晶片上的GaN转移到与GaN具有良好热膨胀匹配的另一模板上。可在很大的硅晶片(大于约6英寸)上制备薄GaN层，同时保持假晶。这将是产生用于未来LED和晶体管工业的6英寸、8英寸或甚至12英寸NPGaN衬底的独特方法。
将薄膜从一个衬底转移到另一衬底的能力具有其它有用的装置应用，例如将NPGaNLED薄膜和晶体管转移到柔性和/或透明衬底。作为另一应用，可将GaN薄层从体HVPE生长的GaN衬底转移。同样地，此方法将是大量生产无位错NPGaN薄膜的简单且便宜的方法。
装置制造方法以及衬底再循环
图13中所显示的另一实施例图解说明将NPGaN用于III-氮化物材料和装置的衬底再循环的概念。使用上文中介绍的新颖电化学工艺，能够形成具有所要孔隙率轮廓的NPGaN层1304。可将纳米多孔结构1304加载回外延室用以退火和再生长。NP区经历转换变成大的气泡或空隙1310。GaN层或装置1312的额外再生长将同时产生包埋高孔隙率区并在热退火期间经历转换1310，其中大的气泡聚结以形成空隙1314。所述空隙促进平面内碎裂、层分离和外延晶片转移。
装置结构1322可生长(例如，使用诸如MOCVD等方法)于NP衬底1320上。装置结构可结合到载体晶片1324并可将组合的装置结构/载体晶片系统1326/1328与NP衬底分离。剩余NP衬底1330可进一步经平滑和回收，以便可重复所述过程。
我们注意到，可在Al2O3(作为LLO替代物)、SiC、Si、GaN和其它衬底上实施相同的概念。此实施例使得用于III-氮化物材料生长和装置制造的衬底能够再循环，此导致成本降低。
在晶片分裂之后剩余表面仍为NP，如先前在图12中所显示。另一实施例提供退火和外延平面化工艺的组合，所述工艺恢复Al2O3上的GaN的平滑度而不需要晶片抛光。所观察到的粗糙度包含高度为0.1微米到0.3微米且区域密度为109cm-2的凸块(mound)。此粗糙度水平类似于标准两步MOCVD工艺中所采用的经粗糙化并转换的LTGaN缓冲层。由于这些小丘和凸块的内在结晶度由最初的GaN下伏层保存，因此高温MOCVD生长期间这些凸块的无缺陷聚结发生1微米到2微米的生长，此使得整个复合结构在EC成孔之前与起始结构相同。
以上所揭示的装置制造实施例提供使用于III-氮化物薄膜生长和装置制造的衬底再循环的简单有效途径，此可显著降低成本同时增强功能性。
所揭示衬底再循环方法的若干经济优点和应用包括以下各项。这些方法可显著减小III-氮化物材料和制造的装置(例如垂直LED)的价格。这些方法同样地适于供与用于生长III-氮化物材料的其它通用衬底(例如蓝宝石、SiC、Si、GaN、A1N等)一起使用。这些方法还能够产生用于电子应用的绝缘体上GaN(GaNOI)结构以及能够产生高质量GaN外延层。
多孔GaN的纳米技术应用
本发明的另一实施例涉及基于NPGaN的纳米晶体的生成。使用先前实施例中所揭示的电化学工艺，可产生具有被极大弱化的机械强度的纤维状单晶GaN材料。机械强度的减小是由于纤维状材料的纵横比的改变和表面积的极大增加。NPGaN对通过超声波(或碾磨)工艺机械碎裂和破裂成荧光标记、光伏打、显示器照明和纳米电子学中所关注的纳米尺寸的纳米晶体更敏感。
用于产生GaN纳米晶体的实施例图解说明于图14a到图14e中。n型GaN层(例如，可为蓝宝石1402或GaN衬底1402上的外延层1406)首先使用上文所揭示的EC蚀刻实施例从顶表面开始成孔化1410。NPGaN的平面SEM图像显示于1418中。将蓝宝石1416上的所得NPGaN1410放置于适宜溶液1426中(例如，包含水、极性或非极性溶液)并超声波处理(在一个实例实施例中，持续约2小时)。超声波处理之后，使用标准技术使表面包含GaN脊和短柱1422。在程序结束时，与澄清透明的去离子水1424相比，液体变得稍混浊1426。
超声溶液中所观察到的混浊是由于GaN纳米晶体(NC)聚集成微米尺寸的微粒，此造成漫反射。图15b显示由许多GaNNC1512和1516构成的此一微粒的TEM图像。图15a中更高放大倍数的TEM图像显示，这些GaNNC1506和1510具有无规取向，此表明最初NPGaN基质已充分碎裂。最后，经干燥的GaN微粒展示特性光致发光发射峰1522和吸收峰1520，如图15c中所显示。
成孔-超声波工艺的另一实施例纳入两阶段电化学蚀刻工艺。EC成孔中需要的特定步骤是产生具有极高孔隙率的包埋层以进行底切并释放上部NPGaN层成隔膜形式，如图16b中所显示和上文中所揭示(图10a-h)。独立式漂浮NPGaN隔膜1610可转移到图17a中所显示的容器中，并超声波处理成微细纳米晶体。这些实施例之间的差别是NPGaN在开始超声波处理时的形式：在先前实施例中，NPGaN是以外延方式附着到衬底，而在图15的实施例中，NPGaN膜/隔膜漂浮在溶液中且对基于超声波处理的碎裂更敏感。这些超声波处理的GaNNC的光学活性可通过当试样被UV光辐照时所发射的可见荧光来观察，如在图17c中所看到。
以上实施例提供生产胶状GaN和InGaN纳米晶体的优良方法。此新技术的经济优点和可能的应用包括(但不限于)：使用纳米晶体制造发光二极管或激光二极管，纳米晶体作为荧光生物标记用于生物医学应用的用途，纳米晶体GaN或InGaN杂合物连同聚合物用光伏打应用的用途，和纳米晶体GaN或InGaN杂合物连同催化金属(如金、镍等)用于能量应用的用途。
另一实施例涉及NPGaN和NPInGaN作为光合过程、水分解和氢产生中的光-阳极或光-阴极的用途。上文已阐述用于产生NPGaN的电化学蚀刻工艺。使用NPGaN或NPInGaN具有以下优点：(1)增强光子吸收，(2)提高光合效率，和(3)减小光电极的降级。
图18图解说明使用NPGaN或InGaN电极1808作为阳极用于水分解试验的试验设备。在此实施例中，首先使用上文所揭示的EC蚀刻程序制造NPInGaN或GaN电极。将此一阳极放置于水1812中并连接到金属(例如，Pt)电极1810，以形成电路。入射到阳极上的太阳能辐射或来自另一源(例如Hg(Xe)灯1806)的辐射驱动电化学反应并引起水分解，同时释放氧1814和氢1815。
使用NP阳极的优点图解说明于图19中所呈现的测量中。使用NP阳极与其中电极不为多孔1902的情况相比使得电流饱和1904极大地减小。NP电极有效的具有较高表面积，此提供光激发载流子将到达半导体/电解液界面的更好的机会，导致更高的转换效率。
总结
应了解，打算使用具体实施方式部分而非发明内容和说明书摘要部分来解释权利要求书。发明内容和说明书摘要部分可列举一个或一个以上但并非发明者所预期的本发明所有实例性实施例或优点，且因此不打算以任何方式限制本发明和所附权利要求书。
特定实施例的上述说明将如此充分地揭示本发明的一般特性，以致于其它人可在不背离本发明的一般概念的情况下无需过多试验即可通过应用所属技术领域中的知识容易地修改及/或调整所述特定实施例以用于各种应用。因此，基于本文所提供的教示和指导，这些调整和修改打算在所揭示实施例的等效物的含意和范围内。应理解，本文的用词或术语是出于说明而非限制目的，因此所属技术领域的技术人员应根据教示和指导来解释说明书中的术语或用词。
本发明的广度和范围不应受任一上述实例性实施例的限制，而应仅根据上文权利要求书和其等价内容来界定。

Claims (10)

1.一种用于生成多孔GaN的方法，其包含：
(a)将GaN暴露于电解质；
(b)将所述GaN耦合到电源的一个端子并将浸于所述电解质中的电极耦合到所述电源的另一个端子以由此形成电路；以及
(c)激励所述电路以增加所述GaN的至少一部分的孔隙率。
2.根据权利要求1所述的方法，其进一步包含施加介于5V与60V范围内的电压，其中所述GaN耦合到所述电源的正端子。
3.根据权利要求1所述的方法，其进一步包含将所述GaN置放在包含蓝宝石、硅、碳化硅或体GaN的衬底上。
4.根据权利要求1所述的方法，其进一步包含在1017cm-3到1019cm-3的范围内掺杂所述GaN的至少一部分，以及提供KOH或HCl作为所述电解质。
5.根据权利要求1所述的方法，其进一步包含在1017cm-3到1019cm-3的范围内掺杂所述GaN的至少一部分，以及提供草酸作为所述电解质。
6.根据权利要求5所述的方法，其进一步包含施加介于5V与60V范围内的电压，其中所述经掺杂GaN耦合到所述电源的所述正端子。
7.根据权利要求5所述的方法，其中所述激励进一步包含控制所施加电压或电流以调整所述GaN孔隙率。
8.根据权利要求5所述的方法，其进一步包含在所述激励之前在所述GaN中形成掺杂轮廓以生成相应的孔隙率轮廓。
9.根据权利要求8所述的方法，其中所述激励进一步包含随时间在介于0V与60V之间的范围内的低值与高值之间控制所施加电压以生成所述孔隙率轮廓。
10.根据权利要求1所述的方法，其进一步包含：
(a)提供草酸作为所述电解质；
(b)将所述GaN耦合到所述电源的所述正端子；以及
(c)施加在介于0V与60V之间的范围内的电压。
CN201610206389.4A 2010-01-27 2011-01-27 用于GaN装置的基于导电性的选择性蚀刻和其应用 Active CN105821435B (zh)

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