CN1463309A - 含镓氮化物块状单结晶在异质基板上的形成法 - Google Patents
含镓氮化物块状单结晶在异质基板上的形成法 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
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Abstract
本发明涉及GaN等含镓氮化物块状单结晶在碳化硅等异质基板上成长的方法,在高加压釜中形成含有碱金属离子的超临界氨溶剂,在该超临界氨中溶解含有镓的供料,在比超临界溶剂中溶解含镓供料时更高温及/或更低压条件下,自溶解上述供料的超临界溶液中将含镓氮化物结晶在以异质基板作为晶种的上,该晶种在组成元素中不含有氧气且a0轴的晶格常数为2.8~3.6。依此,在有导电性基板上可以形成氮化镓系化合物的半导体元件。
Description
技术领域
本发明涉及使超临界溶液在异质基板的晶种上形成结晶,在异质基板上长成含镓氮化物的块状单结晶的方法。
背景技术
应用氮化物的电子光学机器,一般是在堆积的氮化物层与不同蓝宝石基板上或是碳化硅的基板上制造(不定向附晶生长法),最常使用的MOCVD法中,GaN虽是由氨与金属有机化合物来气相成长,但不可能生成块状单结晶层,又,虽然利用缓冲层虽会降低每单位面积的转位数,但目前以上述方法只能降低到108/cm2。
在此,最近,为了降低表面缺陷密度是使用横方向生长法(ELO)。此方法,是在蓝宝石基板上成长GaN层,在其上面再堆积线状或网状的SiO2。针对如此所准备的基板,虽然GaN的横方向成长,可以限制缺陷密度到约107/cm2以下。然而此方法很难降到106/cm2以下。
另外,关于HNP法[″Prospects for high-pressure crystal growth of III-Vnitrides″S,Porowski et.al.,Inst.Phys.Conf.Series,137,369(1998)]中,结晶的成长是在溶解的镓中,毕竟是在液相中进行,会生成10mm左右的GaN结晶。然而,在镓内要得到充分的氮气溶解度,必须要设定温度在1500℃、氮气的压力在15kbar。
为此,为了降低成长步骤的温度与压力,有提议利用超临界氨的议案[″Ammono method of BN,AIN,and GaN synthesis and crystal growth″R.Dwilinski et al.,Proc.EGW-3,Warsaw,June 22-24,1998,MRS InternetJournal of Nitride Semiconductor Research],[″Crystal Growth of galliumnitride in supercritical ammonia″J.W.Kolis et al.,J.Cryst.Growth 222,431-434(2001)],所得的GaN结晶不超过0.5mm程度,因得不到块状单结晶,所以终究不能作为电子零件等的基板。
本发明人,虽提供利用含有付与氨基碱性(ammono-basic)的1种或多数碱化剂的超临界氨溶剂中产生化学输送,可以得到含镓氮化物的单结晶成长方法,但GaN层的转位密度降到106/cm2以下时,导电性机能会下降,就不可能期望其作为电子零件的基板。
发明内容
在此,本发明的第一个目的是提供,在有导电性等机能的异质基板晶种上,可以形成含镓氮化物的块状单结晶的方法。
又,本发明的第二个目的是提供,在品质上可以作为光学元件基板的氮化物块状结晶基板。
为了达成上述目的的本发明第一构成是基于,含有付与氨基碱性(ammono-basic)的一种或多数碱化剂的超临界氨溶剂中不含有氧气的组成成分,a0轴的晶格常数为2.8~3.6的各种结晶构造不容易溶解,产生含镓氮化物的化学输送,可以得到含镓氮化物的单结晶成长,并且为了在比较低温下进行结晶成长,即使使用作为晶种的金属导电性基板,热膨胀差也可以缓和能无障害地进行成长,
在制得含镓氮化物块状单结晶的方法中,其特征为提供,在高压釜内将含镓供料溶解到含有氨与碱金属离子的超临界溶剂中,供给含镓氮化物的溶解度有负温度系数的超临界溶液,自上述超临界溶液利用含镓氮化物的溶解度负温度系数配置在高压釜内,只在a0轴的晶格常数为2.8~3.6的晶种面上选择性的成长含镓氮化物结晶的方法,及在制得含镓氮化物块状单结晶的方法中,其特征为提供,在高压釜内将含镓供料溶解到含有氨与碱金属离子的超临界溶剂中,供给含镓氮化物的溶解度有正压力系数的超临界溶液,自上述超临界溶液利用含镓氮化物的溶解度正压力系数配置在加压釜内,只在a0轴的晶格常数为2.8~3.6的晶种面上选择性的成长含镓氮化物结晶的方法。
依照本发明,因氧气为非构成要素,在超临界氨溶液中不容易溶解,并且a0轴的晶格常数为2.8~3.6,所以GaN(晶格常数3.16)系的含镓氮化物没有不适合的成长。并且在超临界氨中,含镓氮化物的再结晶法因是在比较低温进行结晶成长,即使使用作为晶种的金属导电性基板也可以进行热膨胀差缓和的无障害结晶成长。
具体的是,上述晶种至少有一层表面是可以选自由体心立方结晶系的钼、钨,六方最密充填结晶系的α-Hf、α-Zr,正方晶系钻石,WC构造结晶系WC、W2C,ZnO构造结晶系SiC、尤其α-SiC、TaN、NbN、AlN,六方晶(P6/mmm)系AgB2、AuB2、HfB2,六方晶(P63/mmc)系γ-MoC、ε-MbN等所组成的族群中,也可以是晶种全体是由上述组成所形成。
在第一构成中,进行第二结晶步骤,重点是在晶种面上选择性进行结晶。在此,本案发明的第二构成是含镓氮化物的块状单结晶的结晶方法,其特征是,溶解在含有氨与碱金属离子的超临界溶剂中,将含镓氮化物的溶解度为负温度系数的超临界溶液,至少将高压釜内有a0轴晶格常数为2.8~3.6晶种面的晶种配置在区域中,上升到所定的温度或下降到所定的压力下,超临界溶液的溶解度针对晶种而言的过饱和区域中,调节到不产生自发结晶的浓度以下,只有在高压釜内所配置的晶种面上选择性的成长含镓氮化物结晶。
在上述第二构成中,在高压釜内同时形成所谓的溶解区域与结晶化区域的2个区域时,为了控制针对晶种而言的超临界溶液过饱和,以调整溶解温度与结晶化温度为宜,因此,结晶化区域的温度若设定在400~600℃的温度则能容易控制,在高压釜内溶解温度与结晶化温度的温度差以在150℃以下为宜,较佳是保持在100℃以下则能容易控制。又,针对晶种超临界溶液的过饱和调整,在高压釜内是可以设置1个或多数个阀来区分低温溶解区域与高温结晶化区域,也可以虽然调整溶解区域与结晶化区域的对流量来进行。再,加压釜中形成有特定温度差的溶解区域与结晶化区域2个区域的情形,针对晶种的超临界溶液过饱和调整也可以利用,有提高晶种总面积的总面积GaN结晶当作所投与的含镓供料。
同时,在上述第一构成中,上述碱金属离子为以碱金属或不含卤素物质的碱化剂形状来投与,作为碱金属离子,是选自由Li+、Na+、K+所组成族群中的1种或2种。又,超临界溶剂中所溶解的含镓供料,是含镓氮化物或在超临界溶剂中可溶解可能产生镓化合物的镓前驱体。
又,本发明方法虽是依照氨基碱性反应,但含镓供料者为以HVPE所形成的GaN或化学反应所形成的GaN,即使本来含有氯,对氨基碱性超临界反应也无损害,所以无限制问题。
利用上述第二构成的情形,可以使用由相当于做供料的超临界氨溶剂在平衡反应中溶解的含镓氮化物,与相当于超临界氨溶剂在不可逆反应中溶解的金属镓所组合。
作为上述含镓氮化物,在使用氮化镓时,能容易控制结晶化的反应,在此情形,以使用SiC单结晶作为晶种较佳。
本发明是提供,在上述第一的溶解步骤与第二结晶化步骤的同时,并且在高压釜内进行作为分离方法的第四构成。即提供,得到含镓氮化物的块状单结晶的方法,其特征为在加压釜中形成含碱金属离子的超临界氨溶剂,在该超临界氨溶剂中溶解含镓供料,在比溶解含镓供料时更高温及/或更低压的条件下,自溶解上述供料的超临界溶液将含镓氮化物,在a0轴的晶格常数为2.8~3.6晶种面上结晶的方法。
在第一构成中,在含镓供料的溶解步骤的外,可以另外具备有比超临界溶液更高温及/或更低压中移动的步骤。又,在高压釜中同时形成有温度差的至少2个区域,是由在低温溶解区域中配置含镓供料,在高温结晶化区域中配置有a0轴的晶格常数为2.8~3.6的晶种面晶种来进行。溶解区域与结晶化区域的温度差,必须设定超临界溶液内能确保化学输送的范围内,超临界溶液内的化学输送主要是虽然对流来进行,通常,溶解区域与结晶化区域的温度差是在1℃以上,较佳是在5~150℃,更好是在100℃以下。
本发明中,含镓氮化物的定义如下,以AlxGa1-x-yInyN(0≤x<1、0≤y<1、0≤x+y<1)为对象,因应用途可以含有受与体、接受体或磁性处理剂。超临界溶剂是如以下的定义,含有氨或其衍生物,作为碱化剂者为碱金属离子、至少含有钠或钾的离子,另外,含钾供料主要是由含镓氮化物或其它前驱体所构成,前驱体是含有选自镓的叠氮基、亚胺基、胺基亚胺基、胺基、氢化物、金属间化合物、合金及金属镓,如以下般来定义。
本发明中,晶种有a0轴的晶格常数为2.8~3.6的晶种面,此结晶层中相关表面缺陷密度以在106/cm2以下为宜。具体的,选自体心立方结晶系的钼、钨,六方最密充填结晶系的α-Hf、α-Zr,正方晶系钻石,WC构造结晶系WC、W2C,ZnO构造结晶系SiC、尤其α-SiC、TaN、NbN、AlN,六方晶(P6/mmm)系AgB2、AuB2、HfB2,六方晶(P63/mmc)系γ-MoC、ε-MbN等。
本发明中,含镓氮化物的结晶化虽可以在100~800℃的范围进行,但较好是在300~600℃,更好是可以在400~550℃的温度进行,又,含镓氮化物的结晶化是可以在100~10000bar进行,但较佳是在1000~5500bar,更好是可以在1500~3000bar的压力进行。超临界溶剂内的碱金属离子浓度是,调整到可以确保供料及含镓氮化物的特定溶解度,针对超临界溶液内的其它成分,碱金属离子的莫尔比以控制在1∶200~1∶2,较佳者为1∶100~1∶5,更好为1∶20~1∶8的范围以内为宜。
同时,本发明是有关在含有付与氨基碱性1种或多数碱化剂的超临界氨溶剂中产生化学输送,可得到含镓氮化物的单结晶成长,氨基碱性结晶成长技术,为了认定原本的高技术,在本发明中,所使用的下面用词,是可以用以下的本案说明书来定义其意义。
含镓氮化物是指至少作为构成要件,是至少含有镓与氮原子的化合物,其中至少含有二元化合物GaN、三元化合物AlGaN、InGaN及4元化合物AlInGaN、只要不背离上述氨基碱性结晶成长技术、可改变对镓的其它元素的组合范围。
含镓氮化物的块状单结晶是指虽然MOCVD或是HVPE等的表(epi)成长方法,可以形成如LED或LD的光及电子零件的含镓氮化物单结晶基板。
含镓氮化物的前驱物质是,至少含有镓、主要是含有碱金属、XIII族元素、含氮气及/或氢气物质或是此等的混合物,属于金属镓、此等的合金或金属间化合物、此等的氢化物、胺类、亚胺类、胺基亚胺类、叠氮类,是可以形成在下定义的超临界氨溶剂中溶解的镓化合物。
含有镓的供料是指含有镓氮化物或其前驱物质。
超临界氨溶剂,至少含有氨,超临界氨溶剂为了溶解含镓氮化物,可以理解为含1种或多种碱金属离子。
碱化剂是指在超临界氨溶剂中为了溶解含镓氮化物供给1种或多种碱金属离子,在说明书中有具体例示。
含镓供料的溶解是指上述供料针对超临界溶剂为溶解性镓化合物,例如以镓错体化合物的形态取得可逆性或非可逆性的过程,镓错体化合物与NH3或与其衍生物NH2-、NH2-配位,是以镓为配位中心所围成的错体化合物。
超临界氨溶液是上述超临界氨溶剂与溶解含镓供料所产生的溶解性镓化合物,根据实验,可以发现在充分的高温高压下,固体含镓氮化物与超临界溶液间存在著平衡关系,因此,溶解性含镓氮化物的溶解度,是可以定义为在固体的含镓氮化物存在下,上述溶解性镓化合物的平衡浓度。相关步骤中,此平衡是可以随温度及/或压力的变化而移动。
溶解度的负温度系数是指保持其它全部的参数时,溶解度是以温度的减少系数(monotonically decreasing function)来表示,同样的,溶解度的正压力系数,是指保持其它全部的参数时,溶解度是以压力的增加系数来表示,我们的研究发现,在超临界氨溶剂中含镓氮化物的溶解度至少从300到550℃的温度区域中,自1到5.5Kbar的压力范围内有负的温度系数及正的压力系数。
相对于含镓氮化物的超临界氨溶液的过饱和,是指在上述超临界氨溶液中可溶性镓化合物的浓度为平衡状态的浓度,即,指溶解度更高的意思。在闭锁***中含镓氮化物的溶解情形,如此的过饱和是随溶解度的负温度系数或正压力系数,由增加温度或是减少压力来达成。
超临界氨溶液中有关含镓氮化物的化学输送,是指包括含镓供料的溶解、可溶性镓化合物的经由超临界氨溶液移动、由过饱和超临界氨溶液的含镓氮化物的结晶、等连续步骤,一般化学输送步骤是虽然温度梯度、压力梯度、浓度梯度、溶解的供料与结晶生成物的化学的或是物理的不同性质等的、驱动力来进行。依本案发明方法虽可得到含镓氮化铝的块状单结晶,但上述化学输送是分别在溶解步骤与结晶化步骤的区域中进行,结晶化区域以维持在比溶解区域更高温度来达成较佳。晶种在本案说明书中虽有例示,但也提供进行含镓氮化物的结晶化区域,因其支配结晶的生长品质,所以能选择品质良好。
自发的结晶(Spontaneous crystallization),是指自过饱和超临界氨溶液形成含镓氮化物的核及成长,在高压釜内的任一边都会产生,这是不被期望的步骤,包含在晶种表面的不同方向性的成长(disoriented growth)。对晶种的选择性结晶,是指所谓的非自发性的成长、结晶是在晶种上进行的步骤,为达成块状单结晶成长中不可欠缺的步骤,为本案发明方法之一。
高压釜是指任意形态的为了进行氨碱性结晶成长的闭锁系反应室。又,本发明中所使用的GaN颗粒是指成形GaN粉末状,为招到密度在70%以上,以高密度者为宜。
同时,本案发明实施例中高压釜内的温度分布,因是在没有超临界氨存在下,测定空高压釜,并非实际的超临界温度。又,压力是直接测定的,是由最初导入的氨量、高压釜的温度及容积等来计算决定。
上述方法于实施时,以使用如下的装置为佳,即,本发明是提供其特征为备有产生超临界溶剂的高压釜1的设备、在上述高压釜中设置有对流控制管理装置2、投入备有加热装置5或冷却装置6的炉体4中,的含镓氮化物块状单结晶的生产设备。
上述炉体4,是具有相当于高压釜1的结晶化区域14、备有加热装置5的高温区域,及相当于高压釜1的溶解区域13,备有加热装置5或冷却装置6的低温区域,或是,上述炉体4,是相当于高压釜1的结晶化区域14、备有加热装置5或冷却装置6的高温区域及相当于高压釜1的溶解区域13,备有加热装置5或冷却装置6的低温区域。对流控制管理装置2,是区分成结晶化区域14与溶解区域13,在中心或周围由一张或多张的有孔洞横型阀12所构成。在高压釜1内,是将供料16配置在溶解区域13中,晶种17配置在结晶化区域14中,13与14区域间的超临界溶液的对流是依控制管理装置2来设定构成,其特征为溶解区域13是位在横型阀12的上方,结晶化区域14是位在横型阀12的下方。
附图说明
图1表示在T=400℃与T=500℃中,压力与含有胺化钾(KNH2∶NH3=0.07)的超临界氨内的GaN溶解度关系图。
图2表示实施例1中,p=常数,因时间的变化,高压釜内的温度变化图。
图3表示实施例2中,T=常数,因时间的变化,高压釜内的压力变化图。
图4表示实施例3,于固定容量中,因时间的变化,高压釜内的温度变化图。
图5表示实施例4中,因时间的变化,高压釜内的温度变化图。
图6表示实施例5中,因时间的变化,高压釜内的温度变化图。
图7表示实施例6中,因时间的变化,高压釜内的温度变化图。
图8表示实施例7中,因时间的变化,高压釜内的温度变化图。
图9表示实施例4、5、6、7中所述的高压釜与炉体的剖面图。
图10表示产生含镓氮化物的块状单结晶的设备概要图。
图11表示实施例8中,因时间的变化,高压釜内的温度变化图。
图12表示实施例9中,因时间的变化,高压釜内的温度变化图。
图13表示实施例10中,因时间的变化,高压釜内的温度变化图。
图14表示实施例11,12,因时间的变化,高压釜内的温度变化图。
图15表示实施例13中,因时间的变化,高压釜内的温度变化图。
具体实施方案
在本发明方法中,可以分为供料的溶解步骤,与在晶种面上成长含镓氮化物结晶的高温或是低压条件下移动超临界溶液的步骤。或是,在高压釜中至少分成2个有温度差的区域,可以将含镓供料配置在低温的溶解区域中,晶种配置在高温的结晶化区域中,虽然溶解区域与结晶化区域间的温度差设定在超临界溶液内可以进行对流化学输送的范围,但上述的溶解区域与结晶化区域间的温度差是在1℃以上。含镓氮化物是有AlxGa1-x-yInyN(0≤x<1、0≤y<1、0≤x+y<1),可以含有受与体、接受体或磁性处理剂。超临界溶剂中是可以使用含有碱金属(至少为钾)离子的氨或其衍生物。主要含镓氮化物或是可以使用选自含有叠氮基、亚胺基、胺基亚胺基、胺基、氢化物、含镓的金属化合物或合金、金属镓的GaN前驱体,晶种是至少含有镓或其它族号13(IUPAC、1989)元素的氮化物结晶层,此结晶层的表面缺陷密度是在106/cm2以下。
含镓氮化物的结晶化是在温度为100~800℃、压力100~10000bar的条件下进行。超临界溶剂中碱金属离子的浓度,是可以调整到确保含镓氮化物的适当溶解度,对于超临界溶剂内的其它成分碱金属离子的莫尔比控制在1∶200~1∶2的范围内。
含镓氮化物的单结晶产生设备,是由备有控制对流装置的产生超临界溶剂的高压釜,及高压釜配置有1台或数台备有加热、冷却措施的炉体所组成。在炉体中备有相当于高压釜结晶化区域的加热措施高温区域、与备有相当于高压釜溶解区域的加热、冷却装置的低温区域。或是,可以利用备有加热、冷却装置的高温区域、与备有加热、冷却装置的低温区域的炉体。上述对流控制装置,是区分成结晶化区域与溶解区域,可以在中心或周围制成1个或数个横型阀。高压釜内在溶解区域中配置供料,在结晶化区域中配置晶种。溶解区域与结晶化区域间的超临界溶液对流,是虽然上述的装置来控制。溶解区域位在横型阀的上方,结晶化区域位在横型阀的下方。
依所进行的研究结果,最佳的氮化镓块状单结晶的缺陷密度约为104/cm2,对于表面(0002)的X线测定半值宽,因可得60arcsec以下,所以使用此的半导体元件可以确保适当的品质与寿命特性。
氮化镓在含有碱金属或其化合物(KNH2等)的NH3中,显示出有良好的溶解度。图1所示超临界溶剂内氮化镓的溶解度在400℃到500℃的温度与压力的关系,但此溶解度是定义为莫尔%:SoGaN溶液∶(KNH2+NH3)100%。在此情形的溶剂,是莫尔比XoKNH2∶NH3为0.07的超临界氨内的KNH2溶液。依据上述的图时,溶解度是与压力的增加有关,与温度的减少有关。利用此关系,在溶解度高的条件下进行含镓氮化物的溶解,虽然在溶解度低的条件下结晶,可以成长氮化镓的块状单结晶。此负温度梯度的意思是指在产生温度差的情形,含镓氮化物的化学输送为自低温溶解区域迈向高温的结晶化区域。又,可知其它的镓化合物、金属镓也可以作为GaN错体的供给源使用,例如,在上述成分所成的溶剂中,最简单的原料为金属镓,可以投与Ga错体。其次,适当变化加热等的条件来进行,虽然制造含镓氮化物过饱和溶液,具体的,在选自体心立方结晶系的钼、钨,六方最密充填结晶系的α-Hf、α-Zr,正方晶系钻石,WC构造结晶系WC、W2C,ZnO构造结晶系SiC、尤其α-SiC、TaN、NbN、AlN,六方晶(P6/mmm)系AgB2、AuB2、HfB2,六方晶(P63/mmc)系γ-MoC、ε-MbN等的晶种面上成长结晶。体心立方、面心立方晶的情形是使用以自[1,1,1]方向切出者为宜,以有导电性的α-SiC、Mo、W等为佳。本发明的方法,是在晶种面上可以成长含镓氮化物的块状单结晶,与在由GaN结晶所成的晶种上做成的块状单结晶层得到GaN的化学理论成长有关。上述的单结晶,因是在含有碱金属离子的超临界溶液内成长,因此所得的单结晶也含有0.1ppm以上的碱金属。又,为了防止设备腐蚀需保持超临界溶液的碱性,期望在溶剂中不要投入卤素物质。依本发明的方法,可以用Al或In取代0.05~0.5的Ga。成分可以变更成柔软,可以调整所得氮化物的晶格常数。再,在氮化镓的块状单结晶中,可以接受处理浓度1017~1021/cm3的给予体(Si、O等)、接受体(Mg、Zn等)、磁性物质(Mn、Cr等),虽然接受处理可以改变含镓氮化物的光学、电性、磁性特性。在其它的物理特性中,成长的GaN块状单结晶表面的缺陷密度是可以在106/cm2以下,较佳是在105/cm2以下,更佳是在104/cm2以下。又,对(0002)面的X线半值宽是在600arcsec以下,较佳是在300arcsec以下,更佳是在60arcsec以下成长。最佳的块状GaN单结晶是,可以在缺陷密度为104/cm2以下,对表面(0002)的X线测定半值宽为60arcsec以下成长。
实施例1
使用导入有2台坩釜的容积为10.9cm3的高压加压釜[H.Jacobs,D.Schmidt,Current Topics in Material Science,vol.8,ed.E.Kaldis(north-Holland,Amsterdam,19810,381设计),其中一个配置0.4克以HVPE法所生成的厚度为0.1mm的GaN薄板做供料,另一个是配置α-SiC的晶种,在高压釜中投入0.72克纯度为4N的金属钾。再投入4.81克氨後,紧闭高压釜。将高压釜投入炉中,加热到400℃,高压釜内的压力为2kbar,8天後,温度加热到500℃,压力保持在2kbar状态,再放置8天(图2),操作结果,供料的全量溶解,部分在溶解的晶种上再结晶成GaN层。
实施例2
在容积10.9cm3的高压加压釜中,导入2台坩釜,一个是加入0.44克以HVPE法所生成的厚度为0.1mm的GaN薄板做供料,另一个是配置α-SiC的晶种,在高压釜中投入0.82克纯度为4N的金属钾。再投入5.43克氨後,紧闭高压釜。将高压釜投入炉中,加热到500℃,高压釜内的压力为3.5kbar,2天後,压力降到2kbar,温度保持在500℃的状态,再放置4天(图3),操作结果,供料的全量溶解,在晶种上再结晶成GaN层。
实施例3
在容积10.9cm3的高压加压釜中,导入2台坩釜,一个是加入0.3克纯度6N的金属镓作为供料,另一个是配置α-SiC的晶种,在高压釜中投入0.6克纯度为4N的金属钾。再投入4克氨後,紧闭高压釜。将高压釜投入炉中,加热到200℃,2天後,温度加温到500℃,压力变为2kbar,在此状态下再放置4天(图4),操作结果,供料的全量溶解,在晶种上再结晶成GaN层。
实施例4
在容积35.6cm3的高压加压釜1(图9)中,将1.5克以HVPE法所得的GaN配置在溶解区域13中,α-SiC的结晶配置在结晶化区域14中,投入2.4克纯度为4N的金属钾,其次投入15.9克的氨水(5N),紧闭高压釜1後,投入炉体4中,加热到450℃,高压釜内的压力为2kbar,1天後,结晶化区域14的温度增加到500℃,将溶解区域13的温度降到400℃,在此状态的高压釜1再放置6天(图5)。操作结果,溶解区域13的供料一部分溶解,在结晶化区域14的α-SiC晶种上成长氮化镓。
实施例5
在容积35.6cm3的高压加压釜1(图9)溶解区域13中,配置3.0克GaN颗粒做成的供料,在结晶化区域14中配置α-SiC的结晶,再投入2.4克纯度为4N的金属钾,其次投入15.9克的氨水(5N),紧闭高压釜1後,投入炉体4中,加热到450℃,高压釜内的压力约为2kbar,1天後,将结晶化区域14的温度增加到500℃,溶解区域13的温度降到420℃,在此状态的高压釜再放置6天(图6)。操作结果,溶解区域13的供料一部分溶解,在结晶化区域14的晶种上成长氮化镓。
实施例6
在容积36cm3的高压加压釜1(图9)的溶解区域13中,配置1.6克以HVPE法所得的GaN做成的供料,在结晶化区域14中配置α-SiC的结晶,再加入3.56克纯度为4N的金属钾,其次投入14.5克的氨水(5N),紧闭高压釜1。将高压釜1投入炉体4中,加热到425℃,高压釜内的压力为1.5kbar,1天後,溶解区域13的温度降到400℃,将结晶化区域14的温度增加到450℃,在此状态的高压釜再放置8天(图7)。操作结果,溶解区域13的供料一部分会溶解,在结晶化区域14的α-SiC晶种上成长氮化镓。
实施例7
在容积36cm3的高压加压釜1(图9)溶解区域13中,配置2克以HVPE法所得的GaN做成的供料,加入0.47克纯度为4N的金属钾,在结晶化区域14中配置α-SiC的结晶,其次投入16.5克的氨水(5N),紧闭高压釜1。将高压釜1投入炉体4中,加热到500℃,高压釜内的压力为3kbar,1天後,溶解区域13的温度降到450℃,将结晶化区域14的温度增加到550℃,在此状态的高压釜再放置8天(图8)。操作结果,溶解区域13的供料一部分会溶解,在结晶化区域14的α-SiC晶种上成长氮化镓。
实施例8
在容积35.6cm3的高压加压釜溶解区域中,配置1克以HVPE法所得的GaN做成的供料,在结晶化区域中配置α-SiC的结晶,在高压釜中,加入1.2克纯度为6N的金属镓与2.2克纯度为4N的金属钾,其次投入15.9克的氨水(5N),紧闭高压釜後,投入炉体中,加热到200℃,金属镓的全量溶解做成镓错体的溶液,3日後,温度加热到450℃,高压釜内的压力变为约230MPa,1天後,结晶化区域的温度增加到500℃,溶解区域的温度降到370℃,将此状态的高压釜再放置20天(图11)。操作结果,溶解区域的供料一部分会溶解,在结晶化区域的晶种两面上成长氮化镓单结晶层。
实施例9
在容积35.6cm3的高压加压釜溶解区域中,配置3.0克以GaN颗粒做成的供料,在结晶化区域中配置α-SiC的结晶,再加入2.3克纯度为4N的金属钾,其次投入15.9克的氨水(5N),紧闭高压釜。将高压釜投入炉体中,为了得到由GaN颗粒部分溶解在预备的镓错体中以得到饱和溶液,先加热到250℃,2天後,将结晶化区域的温度增加到500℃,溶解区域的温度增到420℃,在此状态的高压釜再放置20天(图12)。操作结果,溶解区域的供料溶解很多,在结晶化区域的晶种两面上,成长氮化镓层。
实施例10
在容积35.6cm3的高压加压釜1的溶解区域13中,配置0.5克以HVPE法所得的厚度约120mm的GaN板所做成的供料,在结晶化区域14中配置α-SiC的结晶,再加入0.41克纯度为3N的金属钾,其次投入14.4克的氨水(5N),紧闭高压釜後,将高压釜投入炉体中,结晶化区域的温度增加到550℃,溶解区域的温度增加到450℃,得到压力约为2.6kbar,将此状态的高压釜再放置8天(图13)。操作结果,溶解区域的供料一部分会溶解,在结晶化区域的晶种两面上成长氮化镓层。
实施例11
在容积35.6cm3的高压加压釜溶解区域13中,配置0.5克以HVPE法所得的厚度约120mm的GaN板所做成的供料,在结晶化区域14中配置α-SiC的结晶,再在高压釜中,加入0.071克纯度为6N的金属镓与1.4克纯度为3N的金属钠,其次投入14.5克的氨水(5N),紧闭高压釜。将高压釜投入炉体中,加热到200℃,1天後,金属镓溶解,在超临界溶液中,形成溶解性镓,如是,将加压釜的结晶化区域的温度增加到500℃,溶解区域的温度增加到400℃,得到压力约为2.3kbar。在此状态的高压釜再放置8天(图14)。操作结果,溶解区域的供料一部分溶解,在结晶化区域的晶种两面上,成长氮化镓层。
实施例12
在容积35.6cm3的高压加压釜溶解区域13中,配置0.5克以HVPE法所得的厚度约120mm的GaN板做成的供料,结晶化区域14中配置α-SiC的结晶,再于高压釜中,加入0.20克胺化镓与1.4克纯度为3N的金属钠,其次投入14.6克的氨水(5N),紧闭高压釜後,将高压釜投入炉体中,加热到200℃,1天後,胺化镓溶解,在超临界溶液中,形成溶解性镓,如是,将加压釜结晶化区域的温度增加到500℃,溶解区域的温度增加到400℃,得到压力约为2.3kbar,将此状态的高压釜再放置8天(图14)。操作结果,溶解区域的供料一部分会溶解,在结晶化区域的晶种两面上成长氮化镓层。
实施例13
在容积10.9cm3的高压加压釜中,导入2台坩釜,一个是加入0.3克纯度6N的金属镓作为供料,另一个是配置3个α-SiC的晶种,在高压釜中投入0.5克纯度为4N的金属钾。再投入5.9克氨後,紧闭高压釜。将高压釜投入炉中,加热到200℃,压力变为约2.5kbar,1天後,温度加温到500℃,压力保持为在5kbar,在此状态下再放置2天(图15),操作结果,供料的全量溶解,在晶种上再结晶成GaN层。
实施例14
以Mo体心立方晶在[1,1,1]方向切出,代替α-SiC的晶种,使用此作为晶种,其余与实施例1~13相同,在晶种上可以得到GaN结晶的成长。实施例15
以W体心立方晶在[1,1,1]方向切出,代替α-SiC的晶种,使用此作为晶种,其余与实施例1~13相同,在晶种上可以得到GaN结晶的成长。
实施例16
有关本发明的方法,是利用在超临界溶剂内产生含镓氮化物的块状单结晶设备来进行,此设备的主要部分是由生成超临界溶剂的高压釜1,与高压釜1中超临界溶液内可控制化学输送的控制管理装置2所组成,将上述的高压釜1投入备有加热措施5或冷却措施6的(2台)炉体4的室内3中,为了对炉体4保有一定的位置,以带子的固定装置7来固定。炉体4设置在炉床8上,在炉体4与炉床8的周围以钢带9固定,炉床8与炉体4在回转台10上设置,在特定的角度虽然栓固定装置11固定,可以控制高压釜1内的对流种类与对流速度。炉体4中所投入的高压釜1内的超临界溶液对流,可以区分成结晶化区域14与溶解区域13,在中心或周围设定一张或数张有孔洞的横型阀12所组成的对流控制管理装置2。将高压釜1内的两区域温度,虽然设置在炉体4上的控制装置15,设立在100~800℃的范围内,相当于炉体4低温区域的高压釜1内的溶解区域13,是位于横型阀12的上方,在此区域13内配置供料16,相当炉体4高温区域的高压釜内的结晶化区域14,是位于横型阀12的下方,在此区域14中虽配置有晶种17,但将此配置的位置设定在对流的上流与下流为交叉情形的下方。发明的效果
如此所得异质基板晶种,尤其使用有导电特性的α-SiC、Mo及W作为晶种时,在其上所成长的含镓氮化物块状单结晶,因可以具有较好的导电性,同时,有良好的结晶性,所以可以作为各种电子机器的基板、利用氮化物半导体的激光二极体等的光学元件基板。
Claims (19)
1.一种含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:在高压釜中形成含有碱金属离子的超临界氨溶剂、在该超临界氨溶剂中溶解含镓供料、在超临界溶剂溶解含镓供料更高温及/或更低压条件下,由溶解有上述供料的超临界溶液将含镓氮化物,在构成元素中不含氧气且a0轴的晶格常数为2.8~3.6的晶种面上结晶出含镓的氮化物。
2.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中晶种为至少表面是有选自由体心立方结晶系的钼、钨,六方最密充填结晶系的α-Hf、α-Zr,正方晶系钻石,WC构造结晶系WC、W2C,ZnO构造结晶系SiC、TaN、NbN、AlN,六方晶(P6/mmm)系AgB2、AuB2、HfB2,六方晶(P63/mmc)系γ-MoC、ε-MbN等所组成族群的层面。
3.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中在高压釜中同时形成有温度差的至少2个区域,在低温的溶解区域中配置含镓供料,在高温的结晶化区域中配置晶种。
4.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中含镓氮化物是AlxGa1-x-yInyN(0≤x<1、0≤y<1、0≤x+y<1)。
5.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中含镓氮化物可含有受与体、接受体、或磁性处理剂。
6.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中含有晶种的镓氮化物的结晶层中的表面缺陷密度是在106/cm2以下。
7.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中含镓氮化物的结晶是在100~800℃,较佳在300~600℃,更佳在400~550℃的温度下进行。
8.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中含镓氮化物的结晶是在100~10000bar,较佳在1000~5500bar,更佳在1500~3000bar的压力下进行。
9.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中超临界溶剂内碱金属离子的浓度是调整到可以确保供料及含镓氮化物的特定溶解度。
10.根据权利要求1所述的含镓氮化物块状单结晶在异质基板上的形成法,其特征在于:其中相当于超临界溶液内的其它成分的碱金属离子莫尔比控制在1∶200~1∶2,较佳在1∶100~1∶5,更佳在1∶20~1∶8的范围以内。
11.一种含镓氮化物的块状单结晶在异质基板上的形成法,其特征在于:在高压釜中将含镓供料溶解到含氨与碱金属离子的超临界溶剂,供给含镓氮化物的溶解度有负温度系数的超临界溶液,自上述超临界溶液利用含镓氮化物溶解度的负温度系数在高压釜内配置只在构成元素中不含氧气且a0轴的晶格常数为2.8~3.6的晶种面上,选择地成长含镓氮化物的结晶。
12.一种制得含镓氮化物的块状单结晶的方法,其特征在于:在高压釜中将含镓供料溶解到含氨与碱金属离子的超临界溶剂,供给含镓氮化物的溶解度有正压力系数的超临界溶液,自上述超临界溶液利用含镓氮化物溶解度的正压力系数在高压釜内配置只在构成元素中不含氧气且a0轴的晶格常数为2.8~3.6的晶种面上,选择地成长含镓氮化物的结晶。
13.根据权利要求11或12所述的制得含镓氮化物的块状单结晶的方法,其特征在于:其中晶种为至少表面1层是选自由体心立方结晶系的钼、钨,六方最密充填结晶系的α-Hf、α-Zr,正方晶系钻石,WC构造结晶系WC、W2C,ZnO构造结晶系SiC、TaN、NbN、AlN,六方晶(P6/mmm)系AgB2、AuB2、HfB2,六方晶(P63/mmc)系γ-MoC、ε-MbN等所组成族群的层面。
14.根据权利要求11或12所述的制得含镓氮化物的块状单结晶的方法,其特征在于:其中含镓氮化物者是氮化镓。
15.一种含镓氮化物的块状单结晶的结晶方法,其特征在于:在含氨与碱金属离子的超临界溶剂中溶解,将含镓氮化物的溶解度有负温度系数的超临界溶液置于至少在高压釜内的构成元素中不含氧气且a0轴的晶格常数为2.8~3.6有晶种面的晶种所配置的区域中,将上升到所定温度或下降到所定压力,超临界溶液的溶解度在针对上述晶种做成过饱和区域内,调节到不会产生自发性结晶浓度以下後,只在高压釜内所配置的上述晶种面上,选择性成长含镓氮化物的结晶。
16.根据权利要求15所述的含镓氮化物的块状单结晶的结晶方法,其特征在于:其中在高压釜中同时形成溶解区域与结晶化区域的2个区域後,虽然调整溶解温度与结晶温度进行控制对晶种的超临界溶液的过饱和。
17.根据权利要求15所述的含镓氮化物的块状单结晶的结晶方法,其特征在于:其中结晶区域的温度是设定在400~600℃。
18.根据权利要求15所述的含镓氮化物的块状单结晶的结晶方法,其特征在于:其中在高压釜中同时形成溶解区域与结晶化区域的2个区域後,区域间的温度差在150℃以下,最好保持在100℃以下。
19.根据权利要求15所述的含镓氮化物的块状单结晶的结晶方法,其特征在于:其中在高压釜中形成有特定温度差的溶解区域与结晶化区域2个区域,针对构成元素中不含氧气且a0轴的晶格常数为2.8~3.6有晶种面晶种的超临界溶液过饱和调整,是利用投与作为有提高晶种总面积的总面积GaN结晶的含镓供料来进行。
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