CN105931951B - 一种在室温环境下向砷化镓材料引入杂质的方法 - Google Patents
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Abstract
本发明公布了一种在室温环境下向砷化镓材料中引入杂质的方法,是在室温环境下利用惰性气体产生的等离子体处理固态杂质源,使杂质源的原子或离子进入等离子体,这些原子或离子通过与等离子体中正离子和电子碰撞获得动能,进而进入砷化镓材料中。本方法由于不需高温,不仅可以用于砷化镓晶片的掺杂,还可以用于砷化镓器件的掺杂,与传统的高温扩散和离子注入工艺相比,既便捷又经济。
Description
技术领域
本发明涉及半导体技术领域,具体涉及一种在室温环境下向砷化镓材料中引入杂质的方法。
背景技术
砷化镓中杂质对砷化镓的性质有十分重要的影响,离开了杂质,砷化镓很少有什么应用。半导体掺杂工艺在整个半导体工业中具有重要的意义,向纯的砷化镓中引入二族元素铍、镁、锌等杂质会得到p型砷化镓,而向纯的砷化镓中引入六族元素硫、硒等杂质会得到n型砷化镓。在n型砷化镓表面引入受主杂质,或在p型砷化镓表面引入施主杂质都可以得到砷化镓p-n结,它是许多砷化镓器件的基础。将铬掺入砷化镓中,深受主能级位于砷化镓禁带中央附近,因此,在n型砷化镓中掺入铬,由于铬深受主对n型砷化镓中浅施主的补偿作用,可得到电阻率很高的半绝缘砷化镓。半绝缘砷化镓是高速、高频器件及电路、光电集成电路的重要衬底材料。有研究表明,在砷化镓生长过程中掺入一定量的铟,可以使砷化镓晶体中位错密度降低数个量级。
离子注入和高温扩散是半导体掺杂的主要方法。一直到20世纪七十年代,杂质掺杂主要靠高温扩散来完成,在这种掺杂方法中杂质的分布主要是由温度与扩散时间决定。离子注入工艺中掺杂离子以离子束的形式注入到半导体中,杂质分布主要由注入能量和离子种类决定。对于砷化镓的高温扩散掺杂工艺而言,因砷的蒸汽压高,需要采用特定措施来防止砷的蒸发,否则砷和镓数量之比会严重偏离1:1。另一方面,由于离子注入会在砷化镓中造成大量晶格缺陷,消除这些缺陷需要对砷化镓进行退火处理,与前述高温扩散一样,退火过程中的高温会使砷蒸发,须在砷化镓表面加上二氧化硅或氮化硅的保护层后再退火。因此,离子注入和高温扩散给砷化镓的掺杂工艺增加了步骤,降低了工业生产的效率,对砷化镓来说,寻找一种室温掺杂工艺有重要意义。
发明内容
本发明的目的在于提供一种成本低廉、简单便捷的可在室温环境下向砷化镓材料中引入杂质的方法。
本发明的技术方案如下:
一种向砷化镓材料中引入杂质的方法,在室温环境下利用惰性气体产生的等离子体处理固态杂质源,使杂质源的原子或离子进入等离子体,杂质原子或离子与等离子体中正离子和电子碰撞获得动能,进而进入到砷化镓材料中。
具体的,本发明的方法在等离子体发生器的腔体中进行,将固态杂质源放置在等离子发生器腔体中等离子体密度最大的位置,而待掺杂砷化镓材料放置在等离子体密度较小的位置,以惰性气体作为工作气体,在1~2500W功率下进行等离子体处理1~60min。
本发明中待掺杂砷化镓材料可以是砷化镓晶片,也可以是已部分完成的砷化镓器件。优选的,在放置砷化镓晶片或砷化镓器件时,使其待掺杂的那一面面向固态杂质源。
本发明的方法可利用电感耦合等离子体(Inductively Coupled Plasma,简称ICP)发生器进行,也可以利用电容耦合等离子体发生器进行。以ICP设备为例,其具有两套射频电源:一套射频电源叫激励电源,其作用是激活反应室内的工作气体,使之电离,在反应室内产生高密度等离子体;另一套射频电源叫偏压电源,其主要作用是引导离子在垂直于被刻蚀物体方向运动。在利用ICP发生器时,仅使用激励等离子体产生的激励电源,而不使用偏压电源。此外,工作气体使用惰性气体,例如氦气、氩气,而不使用Cl2、CF4等刻蚀气体,因此,掺杂时等离子体对砷化镓材料的表面几乎没有刻蚀作用。
所述固体杂质源例如金片、铝丝、锌锭等等,可以是金属材料,也可以是非金属材料。本发明的方法可以在室温环境下将In、Sn、Zn、Ge、Au、Mn、Al、Mg等金属元素,以及Si、P、C、B、F、S、N等非金属元素引入砷化镓材料中。实验表明,此掺杂方法中引入杂质的数量既与等离子体的密度,即激励射频的功率有关,也和处理时间有关。杂质进入的深度取决于杂质原子本身的性质,等离子体激励射频的功率和处理时间。
上述方法中,作为工作气体的惰性气体常用的有氦气、氩气,进行等离子体处理时工作气体的流量1~100sccm,优选为10~40sccm。
上述方法等离子体处理的功率优选为50~1000W,更优选为100~750W;处理时间优选为2~10min。
在本发明方法中,为了避免将不需要的腔体材料的原子也掺入待掺砷化镓材料中去,在所使用的等离子体发生器腔体中放入两片大尺寸(例如,6吋)的高纯砷化镓片,遮挡等离子体发生器的腔体壁,将固态杂质源和待掺杂砷化镓材料都置于这两大片高纯砷化镓片之间。这两大片高纯砷化镓片不会阻碍等离子体起作用,但可以阻挡腔体原子进入待掺杂砷化镓材料中去。
室温环境下等离子体掺杂的可能的原理如下:
以载气为氦气为例,在等离子体处理过程中,激励射频中的电磁场将电子加速,电子与载气中He原子碰撞,将其离化成He+离子,它和电子构成等离子体。在等离子体中电子温度很高,可达2000-10000K。一方面,等离子中高速运动的正离子和电子轰击杂质源表面,使杂质源表层原子或离子进入等离子体气氛中,并通过碰撞迅速获得动能。另一方面,高速运动的正离子和电子撞击砷化镓材料表面,在其表面产生空位型缺陷。在等离子体处理过程中,这些空位型缺陷会不断释放空位(V)。实验表明,在室温下,空位(V)在砷化镓中就能扩散。为方便书写,在这里,杂质原子M处于砷化镓Ga原子位,记为MGa;M处于砷化镓As原子位,记为MAs。杂质原子处于间隙时记为MI。
在等离子体处理过程中,根据等离子体中的杂质原子或离子体型大小,其进入砷化镓中的方式可分为两种:一种是体型较小的杂质原子或离子可以直接从晶格间隙进入砷化镓中并在间隙中运动;另一种是体型较大的杂质原子或离子首先吸附在砷化镓材料表面,当体内空位移动到吸附杂质原子或离子旁边时,杂质原子或离子就可以跳入空位,并通过后续的空位向体内运动。室温下在完整的砷化镓晶格中,MI的扩散系数大于MGa和MAs的扩散系数,这是因为处于代位的杂质原子或离子的扩散要以近邻存在空位为前提,而MI的扩散不需要此前提。本发明方法在表面引入的空位型缺陷不断释放V,而且室温下V可在砷化镓晶格中快速扩散。当V运动到MGa或者MAs旁边时,MGa或MAs即可进入近邻的V,即从一个格点运动到另一个格点,其扩散系数比完整晶格中的MGa或MAs的扩散系数大大增加。
据文献报道,砷化镓中的杂质原子一般处于代位,取代Ga格点即为MGa,取代As格点即为MAs,最终处于何种代位取决于这些杂质在所处格点时的自由能,杂质原子倾向于自由能较低的位置。
前述通过间隙或空位进入砷化镓中的杂质原子或离子,在初期,其能量远较室温下的热平衡动能为大,经过与晶格原子的多次碰撞,逐渐进入室温下的热平衡状态,即自由能最低的状态。如果杂质原子或离子以间隙状态进入砷化镓,而其热平衡状态是代位,这种杂质原子或离子最终应处于代位,其后续运动借助空位来进行;另外,在热平衡的条件下,一种杂质在砷化镓中的溶解度是一定的,浓度超过溶解度的那部分杂质原子或离子将会分凝出来。
不排除可能存在其它的机制,进一步的机理研究还在进行中。
本发明在室温环境下利用等离子体向砷化镓材料中引入杂质,杂质种类包括金属和非金属。由于本方法在室温环境下实现,与传统的高温扩散和离子注入工艺相比,既便捷又经济。更值得一提的是本掺杂方法中样品表面掺杂浓度较高,并且可同时引进多种杂质。
附图说明
图1.实施例1中等离子体750W 2min掺杂In原子和未作处理的两片相同n型砷化镓中In原子浓度分布的SIMS测量结果。
图2.实施例2中等离子体750W 2min掺杂Sn原子和未作处理的两片相同n型砷化镓中Sn原子浓度分布的SIMS测量结果。
具体实施方式
下面结合实施例对本发明作进一步说明,但不以任何方式限制本发明的范围。
实施例1:
选用液封直拉法生长的n型砷化镓单晶,单面抛光,电阻率106Ω·cm。首先将砷化镓用丙酮、乙醇、去离子水分别进行超声清洗10min。在ICP腔体中,在腔体上方放置纯的砷化镓圆片,腔体底部放置另一片同样大小的纯的砷化镓圆片。将In锭放在底部砷化镓圆片的中心,而将待掺杂的砷化镓样品放置底部砷化镓圆片边缘,样品抛光面朝上。接着对砷化镓片的抛光面进行ICP处理,载气为氦气,流量22sccm,真空度5E-3Pa左右,处理时间2min,功率选用750W。之后利用SIMS手段得到经ICP处理后的砷化镓样品中In杂质浓度随深度的分布,结果如图1所示。由图1可以看出,ICP750W处理后,砷化镓中的In的浓度大大增加,表面浓度达到1019cm-3以上,扩散深度40nm左右,说明该掺杂方法成功地将In杂质引入了砷化镓材料中。
实施例2:
选用液封直拉法生长的n型砷化镓单晶,单面抛光,电阻率106Ω·cm。首先将砷化镓用丙酮、乙醇、去离子水分别进行超声清洗10min。在ICP腔体中,在腔体上方放置纯的砷化镓圆片,腔体底部放置另一片同样大小的纯的砷化镓圆片。将In锭放在底部砷化镓圆片的中心,而将待掺杂的砷化镓样品放置底部砷化镓圆片边缘,样品抛光面朝上。接着对砷化镓片的抛光面进行ICP处理,载气为氦气,流量22sccm,真空度5E-3Pa左右,处理时间2min,功率选用750W。之后利用SIMS手段得到经ICP处理后的样品中Sn杂质浓度随深度的分布,结果如图2所示。由图2可以看出,ICP750W处理后,砷化镓中的Sn的浓度大大增加,表面浓度达到1021cm-3左右,扩散深度40nm左右,说明该掺杂方法成功地将Sn杂质引入了砷化镓材料中。
Claims (10)
1.一种向砷化镓材料中引入杂质的方法,在室温环境下,不对砷化镓材料施加偏置电压的情况下,仅利用惰性气体产生的等离子体处理固态杂质源,使杂质源的原子或离子进入等离子体,杂质原子或离子与等离子体中正离子和电子碰撞获得动能,进而进入到砷化镓材料中。
2.如权利要求1所述的方法,其特征在于,所述方法在等离子体发生器的腔体中进行,将固态杂质源放置在等离子发生器腔体中等离子体密度最大的位置,而待掺杂砷化镓材料放置在等离子体密度较小的位置,以惰性气体作为工作气体,在1~2500W功率下进行等离子体处理1~60min。
3.如权利要求1或2所述的方法,其特征在于,所述砷化镓材料砷化镓晶片或砷化镓器件。
4.如权利要求1或2所述的方法,其特征在于,在进行等离子体处理时,所述砷化镓材料待引入固体杂质的那一面面向固态杂质源。
5.如权利要求1或2所述的方法,其特征在于,所述固态杂质源是金属材料或非金属材料。
6.如权利要求1或2所述的方法,其特征在于,向砷化镓材料中引入的固态杂质选自下列金属元素中的一种或多种:In、Sn、Zn、Ge、Au、Mn、Al和Mg;和/或,选自下列非金属元素中的一种或多种:Si、P、C、B、F、S和N。
7.如权利要求2所述的方法,其特征在于,所述惰性气体是氦气和/或氩气,进行等离子体处理时惰性气体的流量为1~100sccm。
8.如权利要求2所述的方法,其特征在于,等离子处理的功率为50~1000W,时间为2~10min。
9.如权利要求2所述的方法,其特征在于,所述等离子体发生器是电感耦合等离子体发生器或电容耦合等离子体发生器;对于电感耦合等离子体发生器,仅使用其激励电源产生等离子体,而不使用偏压电源。
10.如权利要求2所述的方法,其特征在于,在等离子发生器腔体中放入两片高纯砷化镓片遮挡等离子体发生器的腔体壁。
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