CN101331249B - 掺杂的氮化铝晶体及其制造方法 - Google Patents
掺杂的氮化铝晶体及其制造方法 Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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Abstract
具有高电导率和迁移率的掺杂AlN晶体和/或AlGaN外延层,通过如下步骤进行制造:例如形成包含多种杂质物类的混合晶体,和电激活该晶体的至少一部分。
Description
相关申请的交叉引用
本申请要求于2005年12月2日提交的美国临时申请60/741,701的权利和优先权,这里通过引用将其全部内容并入本文。
政府支持
本发明是借助美国政府支持在国家标准技术研究所(NIST)授予的70NANB4H3051下做出的。美国政府对本发明享有某些权利。
背景技术
半导体材料在宽范围内表现出可控的光和电性能,例如电导率。通过使用掺杂剂实现这样的控制,所述掺杂剂是引入半导体材料的晶格充当电子(负电荷)或空穴(正电荷)源的杂质。可控掺杂使制造各种各样的半导体器件成为可能,例如发光二极管(LED)、激光器、和晶体管。
诸如氮化镓(GaN)和氮化铝(AlN)的氮化物基半导体在技术上受到极大关注,部分是由于它们的宽带隙。这些材料的可控和可复制的掺杂使得制造以短波长(即蓝光、紫光和甚至紫外光波长)发光的发光器件例如LED和激光器成为可能。此外,n型和p型氮化物可以用于制造适合于高功率和/或高温应用的晶体管。在n型半导体中,电子浓度比空穴浓度高得多;因此,电子是多数载流子并支配电导率。相反,在p型半导体中,空穴支配电导率。
通常可能难以制造p型氮化物半导体材料,并且获得具有高Al含量的AlxGa1-xN合金或p型氮化铝(AlN)的导电晶体或外延层已经构成特殊的挑战。向AlN添加碳和氧导致其变成蓝色,这意味着其吸收红光(与不添加杂质的情况下生长的更典型的AlN不同,其由于N空位而倾向于吸收蓝光)。一些导电性测量已表明该蓝色晶体是p型,而其它工作已经令人非常怀疑制造p型AlN的可能性。来自AlN中的大多数替代式掺杂剂的受主能级将趋向于在能带隙中非常深,使得难以实现合理的电导率水平,除非使用高的掺杂剂浓度。遗憾的是,单一p型杂质原子的溶解度往往相当低,并且晶体形成电荷补偿空位缺陷的趋势高。
在任何情况下,迄今为止制造的唯一p型AlN材料涉及在实验室中生长的尺寸只有几毫米(mm)的小晶体。氮化物材料的n型掺杂也存在困难。因此,成功制造大的导电晶体已被证明是另人困惑的。
发明描述
发明简述
本发明有利于形成大尺度(例如,在某些实施方案中,直径为至少1cm)的掺杂AlN晶体。掺杂剂可以是n型和/或p型,并且在电激活之后,该晶体将表现出足够的电导率和/或迁移率特性用以支持商用器件的形成。
依照本发明,通过引入比铝(Al)或氮(N)少一个电子的替代式杂质在完美的化学计量AlN或AlGaN晶格内产生受主能级。诸如N阴离子位置上的空位(表示为VN)或具有额外电子的杂质的电荷补偿缺陷得以理想地避免,但更普遍地其密度减小或者活性较低。为了使用直径几乎与Al或N相同的原子并避免局部应变,优选从元素周期表的上部选择掺杂剂。Al位置的选择包括铍(Be)、镁(Mg)和锌(Zn),而碳(C)是N位置的一个选择。比Al少两个电子的掺杂剂例如锂(Li)也可用来制造p型AlN和AlGaN。
可以通过将例如Be、Mg、Zn、Li或C的单一替代式杂质引入AlN晶格实现AlN和AlGaN的p型掺杂。这种常见的方法被称为单掺杂。其后通常继之以晶体的处理以便电激活杂质物类(species)。
因此,在第一方面中,本发明的特征在于一种形成掺杂AlN晶体的方法,该方法包括:形成包含AlN和多种杂质物类的混合晶体,和电激活至少一部分混合晶体中的至少一种杂质物类。在一个实施方案中,在电激活步骤之前将混合晶体切成多个晶片。电激活步骤之后,掺杂AlN晶体可以在室温下具有大于约10-5Ω-1cm-1、或甚至大于约3×10-3Ω-1cm-1的电导率和/或大于约25cm2V-1s-1的迁移率。
本发明的实施方案可以包括一个或多个以下特征。在电激活之前,混合晶体在室温下的电导率可以小于约10-2Ω-1cm-1,且电激活之后,掺杂AlN晶体可以是n型或p型。所述多种杂质物类可以包括替代式掺杂剂,例如C、O、Be、Mg、Zn或Si。所述多种杂质物类可以包括填隙式掺杂剂,例如Li,并且电激活步骤可以包括下面的至少一种:退火、浸入熔融金属或者向至少一部分混合晶体施加电压。这样的步骤可以导致从至少一部分混合晶体中提取出填隙式掺杂剂。
所述多种杂质物类可以包括至少一种施主和至少一种受主。在一个实施方案中,所述至少一种施主和所述至少一种受主占据阳离子格点。所述至少一种施主包括Si,而所述至少一种受主包括Be、Mg或Zn。在另一实施方案中,所述至少一种施主和所述至少一种受主占据阴离子格点。所述至少一种施主包括O且所述至少一种受主包括C。在各个实施方案中,电激活步骤包括退火。
在另一方面中,本发明的特征在于一种形成p型AlN晶体的方法,该方法包括:形成包含AlN和替代式杂质源的混合晶体,和电激活至少一些替代式杂质。
本发明的实施方案可以包括一个或多个以下特征。所述替代式杂质源可以包括Be3N2。电激活至少一部分替代式杂质的步骤可以包括将Be3N2转变为Be3N3,以及可以包括使混合晶体在氮环境中经受小于约2300℃的温度和小于约100MPa的压力。作为替换或者另外,替代式杂质源可以包括Mg3N2、Zn3N2、Li3N、BeO、BeSiN2、LiBeN、Be2C、BeSiN2、MgSiN2、LiSi2N3、LiMgN或LiZnN中的至少一种。
在又一方面中,本发明的特征在于掺杂的AlN晶体,该掺杂的AlN晶体的厚度为至少约0.1mm,直径为至少约1cm,并且在室温下电导率大于约10-5Ω-1cm-1。在室温下电导率可以大于约3×10-3Ω-1cm-1。所述AlN晶体的迁移率在室温下可以大于约25cm2V-1s-1。直径可以为至少约2cm。所述AlN晶体可以包括选自C、O、Be、Mg、Zn和Si中的至少两种替代式掺杂剂。
在再一方面中,本发明的特征在于一种掺杂的p型AlN晶体,该AlN晶体在室温下的迁移率大于约25cm2V-1s-1。所述AlN晶体可以包括选自C、O、Be、Mg、Zn和Si中的至少两种替代式掺杂剂。
本发明另一方面的特征在于一种掺杂的n型单晶AlN结构,其厚度为至少约0.1mm且直径为至少约1cm。所述AlN结构的迁移率在室温下可以大于约25cm2V-1s-1。所述AlN晶体可以包括选自C、O、Be、Mg、Zn和Si中的至少两种替代式掺杂剂。
在另一方面中,本发明的特征在于一种掺杂的单晶AlN结构,其尺寸为至少2mm×2mm×1mm且在室温下电导率大于约10-5Ω-1cm-1。所述AlN晶体可以包括选自C、O、Be、Mg、Zn和Si中的至少两种替代式掺杂剂。
在另一方面中,本发明的特征在于一种掺杂的p型AlGaN外延层,其具有大于约50%的Al浓度且电导率在室温下大于约10-5Ω-1cm-1。所述电导率在室温下可以大于约3×10-3Ω-1cm-1。所述外延层的迁移率在室温下可以大于约25cm2V-1s-1。在一个实施方案中,所述外延层包括选自C、O、Be、Mg、Zn和Si中的至少两种替代式掺杂剂。
附图简述
在附图中,相同的附图标记在不同视图中通常指代相同的部件。此外,附图并不一定按比例,相反通常着重于说明本发明的原理。在下面的说明书中,参照以下附图描述本发明的各个实施方案,其中:
图1示意绘出了用于单晶AlN生长的晶体生长腔室;
图2是依照本发明的多个实施方案形成掺杂AlN的工艺流程图;和
图3是依照本发明的其它实施方案形成掺杂AlN的工艺流程图。
优选实施方案详述
参照图1,可以通过如美国专利6,770,135所述的升华-再凝结方法形成AlN晶体,通过引用将该专利的全部内容并入本文。晶体生长腔室100包含蒸气混合物110、AlN晶体120和多晶源130,并且被加热炉140包围。在一个实施方案中,晶体生长腔室100包含钨。在替代实施方案中,晶体成长腔室100包含铼钨合金、铼、碳、碳化钽、氮化钽、碳氮化钽、氮化铪、钨与钽的混合物、或其组合,如美国专利申请10/822,336所述,通过引用将该专利申请的全部内容并入本文。
蒸气混合物110由加热晶体成长腔室100一端处的多晶源130产生,并聚结到另一较冷端处的AlN晶体120中。AlN晶体120可以包含有限浓度的填隙式或替代式杂质。在进一步处理时,可以电激活杂质以便掺杂AlN晶体120并向其提供需要的电学性质。在此处描述的所有实施方案中,AlN晶体120还可以包含镓(Ga),使其成为AlGaN晶体。例如,可以将Ga添加到多晶源130使得晶体聚结为AlGaN。在这种情况下,晶体的Al浓度可以大于约50%。AlN晶体120可以具有大于约0.1mm的厚度和大于约1cm的直径。所述直径甚至可以大于约2cm。
图2图解了用于形成p型AlN晶体的工艺200。在步骤220中,在约2000℃至约2300℃的温度下通过升华-再凝结形成AlN晶体120,该晶体是包含AlN和替代式或填隙式杂质源(即至少一种掺杂剂物类)的混合晶体。所述多种替代式杂质的源是Be3N2、Mg3N2、Zn3N2、Li3N、BeO、BeSiN2、LiBeN、Be2C、BeSiN2、MgSiN2、LiSi2N3、LiMgN、LiZnN或其它适宜的材料。相应的替代式杂质包括Be、Mg、Zn、O或其它。化合物Be3N2在约2200℃熔化并在约2250℃下在1巴的N2中分解成液体Be+N2。金属Be在2970℃沸腾。化合物Mg3N2在800-900℃的温度下在1巴的N2中分解。Mg在649℃熔化并在1090℃沸腾。在步骤230中,电激活AlN晶体120内的所述多种替代式或填隙式杂质中的至少一部分。在一个实施方案中,在氮环境中通过高压处理将Be3N2转变为Be3N3,由此电激活Be掺杂剂。可能需要在高达2300℃温度下的高达100MPa的N2压力和高达几个星期的时间。然而,在商业应用中必须考虑到Be的人体毒性。在步骤240中,通过使用线锯或金刚石圆锯将AlN晶体120切成晶片以便直接使用或用于随后在其上的半导体层外延生长和/或器件集成。
还可以通过在生长过程中或生长之后将两种或更多种不同元素引入晶体来实现AlN的掺杂。此处将使用两种元素称为双掺杂;对于三种元素,称为三掺杂。双掺杂方法可以分成两类。
第一类是“非对称双掺杂”(ABD),其中两种杂质代表施主元素和受主元素,并以近似相等的浓度引入。但是,在高浓度下,施主间的相互作用不同于受主之间的相互作用。除孤立的单原子杂质激活能之外,在诸如杂质能带和杂质复合体的多体状态形成中的这种差异是非对称性的来源。施主-受主对优选地具有特殊性质。充当所述多种杂质的源的适宜化合物包括MgSiN2和BeSiN2。在MgSiN2或BeSiN2中,Mg或Be受主占据Al阳离子格点,如同补偿的Si受主那样。因此,它们在晶格中形成最近的相邻对,和净掺杂(以及因此的高电导率)的结果。
在MgSiN2的情形中,施主和受主在高的生长温度下不成对。在高于1018cm-3的掺杂水平下,Mg、Be或Si物类开始形成杂质能带,在该杂质能带中Mg或Be上的空穴可以从一个杂质原子移动到最近的相同杂质原子形成p型次能带(sub-band)。当杂质物类中的一种是Si原子时,Si波函数交叠能形成n型次能带。根据当掺杂剂浓度提高时首先形成哪个次能带,产生的掺杂AlN晶体可以是n型或者p型。优选地,引入浓度大于约1018cm-3的杂质物类,甚至更优选地引入高达2×1022cm-3的浓度。一种适宜的杂质物类源BeSiN2在固态AlN中无限可溶。(参见G.Schneider,L.J.Gauckler,和G.Petzow,J.Am.Ceram.Soc.,Vol.63,P32(1980),通过引用将其全部内容并入本文)。同样,MgSiN2在AlN中具有高的溶解度。由于Si在AlN中是浅施主而Mg是较深的受主,因此用MgSiN2掺杂的AlN通常为n型。
制造p型AlN的ABD方法的另一个例子是将两种不同杂质置于AlN中的N阴离子格点上。这能够通过制造AlN与Al2OC的混合晶体来实现。Al2OC在AlN中的固溶度对于氧和碳都高达3×1022cm-3。参见C.Qui和R.Metselaar,J.Am.Ceram.Soc.,Vol.80,P2013(1997)(“Qui参考文献”),通过引用将其全部内容并入本文。在这种情况下,点缺陷源是Al2O3和Al4C3。气体环境可以包括CO、Al2O、AlCN或这三种气体的各种混合物,且替代式杂质可以包括C和O。
碳由于其低毒性可以优选作为AlN的p型掺杂剂。化合物Al4C3以黄色晶体存在。在惰性的石墨坩埚中,它在2156℃的温度下转熔(peritectically)分解。在高于1500℃的100kPa的N2中,其不存在:Al4C3与N2反应形成AlN和C。可以在碳(石墨)坩埚中在2000℃至2300℃下在100kPa的N2中通过升华-再凝结方法生长AlN晶体。它们生长良好,颜色为黄色,每立方厘米包含几百个小的黑色石墨片,这些石墨片分布在整个晶体中。主要的碳输送蒸气分子是AlCN。当晶体在高温下退火时过量的碳从溶体中脱出。该温度下的生长时间约为150小时。可能因为作为替代式杂质引入N格点的相对少量的C被N空位补偿,因此这些晶体在室温下不导电。
可以通过使用化合物Al2OC非常有效地引入碳作为氮位置上的替代式杂质。化合物Al2OC存在并具有与AlN几乎相同的晶体结构。它在高温下以固态与AlN混溶,Al2OC为0至约40摩尔%。N2和CO分子都包含14个电子。Al2OC的晶体本身不导电。氧杂质作为深施主进入(在氮位置上),并且似乎补偿了较浅的碳受主。成功生长掺有Al2OC的晶体的一个重要因素是在生长过程中或之后对其进行适当的热处理以便得到均匀的体电导率。ABD的这个例子依赖于如下事实:C受主能级显著浅于O施主能级,因此Al2OC化合物在高掺杂浓度下将有效地充当p型掺杂剂。
在一种杂质为替代式而另一种为填隙式的意义上,双掺杂的第二种类型也是非对称的。用于双掺杂AlN的一些有用化合物是LiBeN、LiMgN和LiZnN。元素Be、Mg和Zn将趋向于作为替代式杂质进入AlN晶体,而Li将趋向于成为填隙式杂质。作为填隙式杂质,Li原子在AlN晶格中相对易迁移。因此,可以通过提取出Li离子并将Be留在适当位置来电激活掺杂有LiBeN的AlN晶体,产生p型的导电半导体。可以通过下述进行提取:在真空下加热掺杂的AlN晶体以便蒸发Li、将晶体或晶体切片浸入液态镓(Ga)或铟(In)的熔融金属浴中、或者在外加的直流(DC)电场中使Li漂移到表面。Be受主(或Mg或Zn)要么是孤立的未补偿受主,要么在较高浓度下形成p型次能带。这种制造导电AlN的方法被称为提取-激活双掺杂(EABD)。此外,双掺杂允许将AlN掺杂至非常高的杂质含量水平,这对于独自使用Be、Mg或Zn的单掺杂常常是不可能的。
制造p型AlN的EABD法的另一种应用涉及制造具有化合物LiSi2N3的AlN混合晶体。然后,如上文所述提取出Li(在这种情形中Li为Al阳离子格点上的替代式杂质)以便留下掺杂有VAlSi2N3(即对于每个Al空位,Al位置上有两个Si原子)的AlN晶体。这使晶体成为净P型半导体。但是,应该注意在这个工艺期间避免退火除去过多的铝空位(VAl)(例如进行至过高的温度),因为掺杂有VAlSi3N4(即每个VAl三个Si原子)的晶体将被完全补偿并且在低掺杂浓度下不导电。
图3图解了用于形成掺杂AlN晶体的替代工艺300。在步骤320中,在约2000℃至约2300℃的温度下通过升华-再凝结形成AlN晶体120——包含AlN和多种杂质物类(即不同类型的掺杂剂原子)的混合晶体。所述杂质物类可以包括诸如C、O、Be、Mg、Zn和Si的替代式掺杂剂和/或诸如Li的填隙式掺杂剂。可以通过如下方式引入所述杂质物类:利用例如MgSiN2、BeSiN2、Al2OC、LiBeN、LiMgN、LiZnN或LiSi2N3的化合物(即一种或多种杂质物类的源)作为多晶源130的一部分,或者将其气态前体引入蒸气混合物110中使得AlN晶体120包含目标化合物和/或杂质物类。这时,在电激活之前,AlN晶体120可以具有低的电导率,例如在室温下小于约10-2Ω-1cm-1,因为所述多种杂质物类可以相互补偿。AlN晶体120的电导率甚至可以小于约10-5Ω-1cm-1。
为了在AlN中的N阴离子位置上获得非常高的C浓度,可以用0.1-50摩尔%的Al2OC和99.9-50摩尔%的AlN制造混合多晶材料。然后使用所述混合多晶材料作为用于生长掺杂AlN晶体的多晶源130。可以通过将适当比例的AlN和Al2OC粉末混合并烧结来形成所述混合多晶源材料。但是,纯净的Al2OC结构相当不稳定,并且通过制造其与AlN的混合晶体使其最佳稳定。这可以在利用Al4C3、AlN和Al2O3的热力学性质的仔细控制的条件下进行。
制造AlN-Al2OC多晶材料的一种此类方法是将Al2O3粉末添加到Al-N-C混合物(具体地说,要么(i)AlN+C粉末,要么(ii)AlN、C和Al粉末,要么(iii)AlN和Al4C3粉末)并将其加热以便将相对高浓度的Al2OC并入AlN。该反应优选在1700℃-2000℃的温度范围内进行,这时Al2OC是热力学稳定的(参见例如Qui参考文献和Y.Larrere等人的Rev.Int.Hautes Temp.Refract.Fr.,Vol.21,P3(1984),通过引用将其全部内容并入本文)。我们可以计算出在2000℃稳定的最高压力约为1巴。可以将Al2O3加Al-N-C粉末冷压,然后在最高达1990℃的温度下在顶部带螺纹的石墨圆筒中烧结。然而,烧结将产生略微多孔的样品,因此更好在约1900℃的温度下在紧密密封的石墨模中热压粉末持续2-3小时。所述密封防止气体从压模中泄漏出从而改变化学组成。反应热压的使用利用了Al2O3与Al4C3的反应中5%的体积收缩来形成Al2OC。理想地在压力下冷却混合物以防止逆反应。热压产生>98.5%理论密度的样品,如S.Y.Kuo和A.V.Virkar的J.Am.Ceram.Soc.,Vol.73,P2640(1990)中所示,通过引用将其全部内容并入本文。
具有掺杂多晶材料的AlN晶体生长的理想进行应注意晶体生长腔室100的类型。例如,使用AlN-Al2OC多晶起始材料时,可以优选使用由TaC或石墨(C)制成的晶体生长腔室100。
在一个实施方案中,所述多种杂质物类包括至少一种施主和至少一种受主。此外,这样的杂质物类对可以占据AlN晶格中的阳离子或阴离子格点。例如,化合物Al2OC可以充当施主物类O和受主物类C的源,它们两者都占据阴离子(N)格点。相反,诸如BeSiN2、MgSiN2和ZnSiN2的化合物可以充当施主物类Si和受主物类Be、Mg和Zn的源,它们全部占据阳离子(Al)格点。
继续参照图3,在步骤320中还可以引入填隙式和替代式杂质物类的组合。例如,诸如LiBeN、LiMgN或LiZnN的化合物可以提供Li作为填隙式杂质以及诸如Be、Mg、Zn或Si的物类作为替代式杂质。在这种情况下,存在填隙式杂质和替代式杂质两者可以使AlN晶体120基本为本征性直到在随后的步骤340中提取出填隙式杂质(如下所述)。另一个例子是LiSi2N3掺杂,其中Li和Si两者都将是Al阳离子位置上的替代式杂质。因此,AlN晶体120可以具有低的电导率,例如在室温下小于约10-2Ω-1cm-1,直到在随后的步骤340中提取出更加易于迁移的替代式Li杂质(如下所述)。在这个阶段,AlN晶体120的电导率甚至可以小于约10-5Ω-1cm-1。
在一个实施方案中,O杂质的源是Al2O3,它向AlN晶体120提供Al空位和替代式O形式的点缺陷。该Al2O3点缺陷源提供Al空位,因为Al2O3实际是以Al2VAlO3溶解,其中VAl表示一个Al空位。在2300℃的生长温度和低的Al2O3浓度下,O原子将随机分布在N位置上,而Al空位随机分布在Al位置上。在缓慢冷却过程中,O原子可以趋向于簇集在Al空位周围,因为它们的直径比N原子略大,导致应力消除的簇集。可以通过在30分钟或更少的时间内将晶体从生长温度快速冷却来预防这种簇集。快速冷却将导致在N阴离子格点和Al空位上具有未簇集的O点缺陷的AlN晶体。
在可选步骤330中,将此刻包含至少一种杂质物类的AlN晶体120切成晶片。在可选步骤335中,在AlN晶体120的至少一个晶片上沉积外延层。所述外延层可以包括AlN、GaN、InN或其合金或混合物。所述外延层的Al浓度可以大于50%。(因此,对于AlxGa1-xN外延层,x可以大于0.5)。在步骤335期间,所述外延层可以掺杂有至少一种杂质物类,例如O。所述外延层的厚度可以为约0.5微米(μm)至200μm。在步骤340中,电激活至少一部分AlN晶体120(该晶体此刻可选为晶片形式)中(和/或沉积在其上的外延层中)的至少一种杂质物类,以便形成掺杂晶体。在电激活之后,所述晶体(和/或沉积在其上的外延层)可以具有净的n型或p型掺杂水平。可以通过例如在约2000℃至约2300℃的温度范围内对AlN晶体120进行退火来实现电激活。
在步骤320中已经引入填隙式杂质物类时,步骤340可以包括方法:提取出填隙式杂质物类,同时将一种或多种激活的替代式杂质物类留在AlN晶体120中。在这样的实施方案中,步骤340可以包括:在高于300℃但低于1600℃的温度下(以避免过度损伤AlN基质晶体)在真空中对AlN晶体120进行退火以蒸发填隙式杂质物类,将AlN晶体120或其晶片浸入液态镓(Ga)或铟(In)熔融金属浴中,或向AlN晶体120施加电压以便使填隙式杂质物类漂移到表面。
步骤340可以包括在可以向AlN晶体120提供至少一种附加杂质物类的环境中退火。在一个实施方案中,AlN晶体120在约2000℃至约2300℃的温度范围内退火。在O杂质的情形中,选择温度以便防止簇集或使O-VAl簇再溶解。所述环境是例如30巴下的90%N2+10%CO的气氛,退火时间为例如24小时,且越厚的晶片需要越长的时间。一些CO扩散到晶体中,而一些氮和氧扩散出。因此,退火步骤将C(一种附加的杂质物类)并入AlN晶体120。类似地,如果AlN晶体120的晶片上存在外延层,这样的退火可以向外延层提供附加的杂质物类。因此,所述外延层可以包含多种杂质物类,其中至少一种被电激活。
一旦步骤340完成,AlN晶体120和/或沉积在其上的外延层就可以具有理想的电特性。这些电特性包括例如电导率在室温下大于约10-5Ω-1cm-1,或者在室温下甚至大于约3×10-3Ω-1cm-1。电导率在室温下甚至可以大于约0.1Ω-1cm-1。AlN晶体120和/或沉积在其上的外延层的迁移率在室温下可以大于约25cm2V-1s-1。
结果是四元晶体,该四元晶体主要为AlN但在N格点上具有高浓度的O和C。由于过量的O,其还将具有一定浓度的Al空位(VAl)。在缓慢冷却过程中,一些过量O可能再次簇集在Al空位周围,但迁移性比O原子差的C原子不会。在溶体中C位于并停留在N位置上,并且C浓度与O浓度相当或者大于O浓度。现在AlN晶体120是良好的p型导体(室温下电导率σ>3×10-3Ω-1cm-1)。在优选实施方案中,AlN晶体120在室温下的迁移率大于25cm2V-1s-1,因为高浓度的C产生非定域的受主能带,而由O产生的较深施主能级保持为定域性。优选的AlN晶体的尺寸超过2mm×2mm×1mm,并且室温下的电导率大于10-5Ω-1cm-1。
该p型掺杂剂的激活能将取决于其浓度,但是由于Al2OC和Al2VAlO3两者在AlN中的高溶解度,因而有可能制造退化掺杂的p型AlN以及轻掺杂的材料。希望C浓度超过约1×1018cm-3以便实现实用的p型导电性。使用这种技术能够获得非常高的C浓度(最高达约2×1022cm-3),并且这样的浓度有助于获得高的p型掺杂水平(和较高的导电性)。
Al2O3和CO掺杂以及退火处理对于控制p型掺杂存在通常重要。在优选实施方案中,O与C的原子比约为一比一(1∶1),且大部分C被激活。如果存在比此更多的O,则将有较少的C中心被激活,而较低的O浓度可以导致C析出并且为非电活性。
可以看到,本文描述的方法为包括AlN和AlGaN的掺杂晶体和外延层的制备提供了基础。此处使用的术语和措辞用作描述而非限定性的术语,在这些术语和措辞的使用中并不意图排除所示和所述特征的任何等效物或其部分。相反,认为在本发明权利要求范围内可以做各种修改。
权利要求如下:
Claims (24)
1.形成掺杂AlN晶体的方法,该方法包括以下步骤:
a.形成包含AlN和多种杂质物类的混合晶体,所述多种杂质物类由源化合物提供;和
b.优先电激活至少一部分混合晶体中的一种杂质物类以便形成掺杂AlN晶体。
2.如权利要求1所述的方法,该方法还包括在电激活步骤之前将混合晶体切成多个晶片的步骤。
3.如权利要求1所述的方法,其中在电激活步骤之后,该掺杂AlN晶体在室温下具有大于10-5Ω-1cm-1的电导率。
4.如权利要求3所述的方法,其中在电激活步骤之后,该掺杂AlN晶体在室温下具有大于3×10-3Ω-1cm-1的电导率。
5.如权利要求1所述的方法,其中在电激活步骤之后,该掺杂AlN晶体在室温下具有大于25cm2V-1s-1的迁移率。
6.如权利要求1所述的方法,其中在电激活步骤之前,该混合晶体在室温下具有小于10-2Ω-1cm-1的电导率。
7.如权利要求1所述的方法,其中在电激活步骤之后,该掺杂AlN晶体为n型。
8.如权利要求1所述的方法,其中在电激活步骤之后,该掺杂AlN晶体为p型。
9.如权利要求1所述的方法,其中所述多种杂质物类包括替代式掺杂剂。
10.如权利要求9所述的方法,其中该替代式掺杂剂选自C、O、Be、Mg、Zn和Si。
11.如权利要求1所述的方法,其中所述多种杂质物类包括填隙式掺杂剂。
12.如权利要求11所述的方法,其中该填隙式掺杂剂包括Li。
13.如权利要求11所述的方法,其中电激活步骤包括下述中的至少一种:退火、浸入熔融金属和向混合晶体的至少一部分施加电压。
14.如权利要求13所述的方法,其中该电激活步骤从至少一部分混合晶体中提取出填隙式掺杂剂。
15.如权利要求1所述的方法,其中所述多种杂质物类包括至少一种施主和至少一种受主。
16.如权利要求15所述的方法,其中所述至少一种施主和所述至少一种受主占据阳离子格点。
17.如权利要求16所述的方法,其中所述至少一种施主包括Si,且所述至少一种受主包括Be、Mg或Zn。
18.如权利要求15所述的方法,其中所述至少一种施主和所述至少一种受主占据阴离子格点。
19.如权利要求18所述的方法,其中所述至少一种施主包括O,且所述至少一种受主包括C。
20.如权利要求1所述的方法,其中所述电激活步骤包括退火。
21.如权利要求20所述的方法,其中在包含附加杂质物类的环境中进行退火。
22.形成p型AlN晶体的方法,该方法包括以下步骤:
a.形成包含AlN和替代式杂质源的混合晶体;和
b.电激活至少一些替代式杂质以便形成p型AlN晶体;
其中所述替代式杂质源包括Be3N2、Mg3N2、Zn3N2、Li3N、BeO、BeSiN2、LiBeN、Be2C、BeSiN2、MgSiN2、LiSi2N3、LiMgN或LiZnN中的至少一种。
23.如权利要求22所述的方法,其中所述替代式杂质源包括Be3N2,并且所述电激活步骤包括将Be3N2转化为Be3N3。
24.如权利要求22所述的方法,其中所述电激活步骤包括在氮环境中使混合晶体经受小于100MPa的压力和小于2300℃的温度。
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CN101331249A (zh) | 2008-12-24 |
JP5312664B2 (ja) | 2013-10-09 |
US10692980B2 (en) | 2020-06-23 |
US20070131160A1 (en) | 2007-06-14 |
JP5281408B2 (ja) | 2013-09-04 |
WO2007065018A3 (en) | 2007-08-02 |
US20170084702A1 (en) | 2017-03-23 |
US10068973B2 (en) | 2018-09-04 |
US20190035898A1 (en) | 2019-01-31 |
JP2013032287A (ja) | 2013-02-14 |
JP2013155112A (ja) | 2013-08-15 |
US20100187541A1 (en) | 2010-07-29 |
WO2007065018A2 (en) | 2007-06-07 |
US11183567B2 (en) | 2021-11-23 |
US20200350411A1 (en) | 2020-11-05 |
JP2009518263A (ja) | 2009-05-07 |
EP1954857A2 (en) | 2008-08-13 |
US8747552B2 (en) | 2014-06-10 |
JP5436710B2 (ja) | 2014-03-05 |
US9525032B2 (en) | 2016-12-20 |
EP1954857B1 (en) | 2018-09-26 |
US20140231725A1 (en) | 2014-08-21 |
US7641735B2 (en) | 2010-01-05 |
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