CN103700743A - 一种发光二极管及其缓冲层的制备方法 - Google Patents
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Abstract
本发明公开了一种发光二极管及其缓冲层的制备方法,所述发光二极管包括:蓝宝石衬底,依次形成于蓝宝石衬底上的缓冲层、N型半导体层、有源发光层、P型半导体层,所述的缓冲层材料为InxGa1-xN,在整个外延缓冲层生长过程中,缓冲层中In、Ga的含量处于梯度变化的过程,x是不断变化的过程,x从开始的1到缓冲层生长结束时为0,即缓冲层中In的量是不断递减的过程,Ga的量是不断递增的过程。
Description
技术领域
本发明属于发光二极管元件领域,涉及一种发光二极管,对缓冲层结构进行了改进,及其缓冲层的制备方法。
背景技术
随着近年来全球绿色环保、节能安全意识的不断提高,各类节能环保产品被广泛关注,其中发光二极管(LED)的推广应用备受重视。发光二极管是一种将电能转化为光能的发光器件,主要应用于照明、显示、指示、装饰领域。随着全世界节能环保意识的不断提高,发光二极管凭借其拥有“比节能灯还节电80%”的良好性能,近年来越来越多地被广泛运用,很多国家已经开始取代白炽灯。
随着发光二极管的不断应用发展,目前如何克服其技术缺陷倍受关注,其中最主要的是在外延生长过程中磊晶层与衬底之间的晶格常数失配问题,导致发光二极管出光率低下及使用寿命远低于理论值。为此在外延生长的过程中,衬底及磊晶层材料、工艺的选择被列为重中之重,在衬底选取过程中,蓝宝石主要成分是氧化铝(Al2O3),属于三方晶系,具备对称形六方体结构,2050℃熔点,1900℃的工作温度,热稳定性很好,另外其机械强度高,易于处理和清洗,被大多数工艺选为磊晶衬底。但考虑蓝宝石衬底与GaN基晶格失配严重,先在衬底上生长一层缓冲层(又称晶核形成层)的技术被提出,于是,各种各样的缓冲层被研制出来,缓冲层的晶格常数与衬底之间必须相接近,以此才能提供成核位置,便于其他各层的生长,形成相同的晶体结构,提升发光二极管的结晶度。缓冲层生长制备过程中,其材料的选取,制备工艺的筛选,直接影响后续各层的质量,对发光二极管的出光率及使用寿命起决定性作用。
发明内容
为解决氮化镓系与蓝宝石衬底之间晶格匹配不佳问题,减少缺陷密度,本发明的发明人通过在现有技术基础上,对缓冲层经过无数次改进试验后发现,当在外延磊晶时缓冲层以InxGa1-xN结构取代低温GaN,其在生长过程中如果里面的组成成分处于梯度渐变时,其能使缓冲层与衬底之间、缓冲层内部、缓冲层与N型半导体层之间进行很好的衔接,解决他们之间的晶格失配问题,减少他们之间因晶格匹配度问题所致的缺陷。
本发明的缓冲层由InxGa1-xN组成,其中In、Ga的含量在缓冲层生长过程中呈梯度变化,沿蓝宝石衬底往上x为递减,即在缓冲层中In的含量从下至上递减,Ga的含量从下至上递增,0≤x≤1。通过氮化铟镓组分渐变的过程,将晶格大小由蓝宝石过度至氮化镓,减少蓝宝石衬底与氮化镓材料晶格失配的问题。但在氮化铟镓生长过程中由于氮化镓与氮化铟晶格失配度达到10%,铟原子半径大于镓的原子半径,铟的元素蒸汽压比镓高,铟原子键能较低,易挥发,等等,使得氮化铟镓在生长过程中面临诸多问题,铟原子很难引入,要使铟、镓原子能梯度分布难上加难。为解决这系列问题,本发明的发明人在缓冲层生长过程中控制其生长温度以450℃-800℃之间为主,优选500℃-600℃之间,反应腔体压力为50-760torr之间,优选300-450torr之间,利用氮气作为主要载气,氨气作为反应气体,三甲基镓(TMGa)和三甲基铟(TMIn)生长InxGa1-xN缓冲层,当缓冲层生长至其总厚度¾时,生长温度开始持续升高,直至900-1100℃,优选1100℃,载气由氮气转化为氢气,缓冲层中IN的含量逐渐降为0,缓冲层以GaN为收尾。停止通入反应气体一段时间,使缓冲层表面过剩的In挥发,保证缓冲层中In梯度变化。缓冲层厚度控制在100Å至1000Å之间,优选200Å至400Å之间,更优选为300Å。
本发明制备铟、镓组份梯度变化的InxGa1-xN缓冲层的方法如下:
第一步,在生长前,调节TMIn的流量在(300±10%)cc.mole/min, TMGa的流量为0mol/min。反应温度调节至450℃-800℃之间,腔体压力为50-760torr之间。选择氮气为载气,氨气为反应气体。
第二步,保持反应温度、压力等反应条件不变,使TMIn的流量不变,开始通入TMGa,其流量由0mol/min匀速增加,待缓冲层生长至其总厚度1/4时,TMGa流量至(300±10%)cc.mole/min。
第三步,保持反应温度、压力等反应条件不变,控制TMIn的流量匀速降低,待缓冲层生长至其总厚度3/4时,TMIn的流量至原流量的1/4。TMGa的流量保持不变。
第四步,保持其他反应条件不变,匀速提高反应温度,控制其当缓冲层生长完成时至900-1100℃,同时此过程保持TMIn的流量在第一步、第二步中流量的1/4不变,TMGa的流量保持不变,载气由氮气转变为氢气,其变化速度是均匀的,控制在当缓冲层生长完成时,载气完全转变成氢气。
第五步,缓冲层生长结束,保持现有反应条件不变,但停止通入TMIn、TMGa,使缓冲层表面过剩的In挥发,保证缓冲层中In梯度变化。
缓冲层反应生长过程中TMIn的流量、TMGa的流量、生长温度变化曲线示意图见附图1-3。
附图说明
本发明中附图仅为了对本发明进一步解释,不得作为本发明发明范围的限制。
附图1 缓冲层生长反应温度曲线示意图
附图2 缓冲层生长TMIn流量曲线示意图
附图3 缓冲层生长TMGa流量曲线示意图
具体实施方式
本发明的实施例仅为对本发明进行解释,便于本领域普通技术人员能根据本发明内容能实施本发明,不得作为本发明发明范围的限制。
实施例
1
在蓝宝石衬底上生长厚度为400Å的铟、镓组份梯度变化的InxGa1-xN缓冲层,在外延生长前,调节温度为550℃,压力为400torr,以氮气为载源气体,氨气为反应气体,调节TMIn流量为300cc.mole/min,保持反应温度、压力等反应条件不变,控制TMIn的流量不变,开始通入TMGa,其流量由0cc.mole/min开始匀速增加,控制缓冲层生长至缓冲层总厚度1/4时,TMGa的流量达到300 cc.mole/min,此时开始降低TMIn的流量匀速降低,当缓冲层生长至其总厚度3/4时,TMIn的流量降至原流量的1/4,过程中TMGa的流量保持300 cc.mole/min不变,维持TMIn、TMGa此时的流量,在缓冲层总厚度最后1/4的过程中,匀速提高反应温度控制缓冲层生长结束时温度至1100℃,缓冲层总厚度最后1/4的过程中,载气由氮气匀速转变成氢气,控制缓冲层生长结束时载气只有氢气。缓冲层生长结束后保持温度为1100℃,压力为400torr,停止通入TMIn、TMGa,使缓冲层表面过剩的In挥发。
实施例
2
在蓝宝石衬底上生长厚度为250Å的铟、镓组份梯度变化的InxGa1-xN缓冲层,在外延生长前,调节温度为580℃,压力为350torr,以氮气为载源气体,氨气为反应气体,调节TMIn流量为310cc.mole/min,保持反应温度、压力等反应条件不变,控制TMIn的流量不变,开始通入TMGa,其流量由0cc.mole/min开始匀速增加,控制缓冲层生长至缓冲层总厚度1/4时,TMGa的流量达到295 cc.mole/min,此时开始降低TMIn的流量匀速降低,当缓冲层生长至其总厚度3/4时,TMIn的流量降至原流量的1/4,过程中TMGa的流量保持295 cc.mole/min不变,维持TMIn、TMGa此时的流量,在缓冲层总厚度最后1/4的过程中,匀速提高反应温度控制缓冲层生长结束时温度至980℃,缓冲层总厚度最后1/4的过程中,载气由氮气匀速转变成氢气,控制缓冲层生长结束时载气只有氢气。缓冲层生长结束后保持温度为980℃,压力为350torr,停止通入TMIn、TMGa,使缓冲层表面过剩的In挥发。
Claims (7)
1.一种发光二极管,其依次包括蓝宝石衬底、缓冲层、N型半导体层、有源发光层、P型半导体层,其特征在于缓冲层为InxGa1-xN,沿蓝宝石衬底往上x为递减,即在缓冲层中In的含量从下至上递减,Ga的含量从下至上递增,0≤x≤1。
2.
根据权利要求1所述的发光二极管,其特征在于该缓冲层的厚度在100Å至1000Å之间。
3.
根据权利要求1所述的发光二极管,其特征在于该缓冲层的厚度在100Å至1000Å之间。
4.
根据权利要求1所述的发光二极管,其特征在于该缓冲层的厚度为300Å。
5.
权利要求1-4各项所述的发光二极管的缓冲层的制备方法,其特征在于MOCVD反应室中生长缓冲层的压力为50-760torr, 载源气体为氮气,反应气体为氨气,开始时温度控制在450℃至800℃之间,TMIn的流量控制在300±10%cc.mole/min,TMGa的流量由0 cc.mole/min开始匀速增加,直至缓冲层生长至缓冲层总厚度的1/4时,TMGa的流量达到300±10%cc.mole/min,并维持此流量,开始匀速降低TMIn的流量,至缓冲层生长至缓冲层总厚度的3/4时,TMIn的流量降低至原流量的1/4,维持此流量,同时TMGa的流量仍然不变,其生长温度开始匀速升高,载气由氮气匀速转变成氢气,当缓冲层生长结束时其温度为900-1100℃,载气完全为氢气。
6.
根据权利要求5所述制备方法,其特征在于MOCVD反应室中生长缓冲层的压力为300-450torr,开始时温度控制在500℃至600℃之间,载源气体为氮气,当生长至缓冲层总厚度的3/4时,其生长温度开始匀速升温,载气由氮气匀速转变成氢气,当缓冲层生长结束时其温度为1000-1100℃,载气为氢气。
7.
根据权利要求5所述的制备方法,其特征在于开始时其在MOCVD反应室中生长缓冲层的温度控制在550℃,当生长至缓冲层总厚度的3/4时,其生长温度开始匀速升温,当缓冲层生长结束时其温度为1100℃。
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