CN117512559A - 一种原位c掺杂的p型六方氮化硼薄膜及其制备方法 - Google Patents
一种原位c掺杂的p型六方氮化硼薄膜及其制备方法 Download PDFInfo
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Abstract
一种原位C掺杂的P型六方氮化硼薄膜及其制备方法，属于半导体薄膜制备和掺杂技术领域。本发明采用低压化学气相沉积(LPCVD)技术，通过BCl3+NH3→hBN+HCl反应在衬底上生长本征hBN薄膜缓冲层，然后在缓冲层上以Cp2Mg为掺杂源进行原位掺杂，受控降温后得到原位C掺杂的P型六方氮化硼薄膜。薄膜的生长速率与厚度可通过生长温度、生长源流量等进行调控，其电学性质与掺杂浓度可通过掺杂源加热温度与稀释比例进行调节。本发明所述方法简单稳定且掺杂均匀，能够制备出空穴浓度较高的P型hBN薄膜，进一步通过异质外延等方式，可以与其他半导体材料形成各种半导体器件。
Description
技术领域
本发明属于半导体薄膜制备和掺杂技术领域，具体涉及一种原位C掺杂的P型六方氮化硼薄膜及其制备方法。
背景技术
近年来，氮化物半导体材料与器件发展迅速，已经成为紫外光电器件、功率电子器件等领域不可或缺的一部分。六方氮化硼(hBN)是一种人工合成的Ⅲ-Ⅴ族化合物，具有与石墨类似的六方层状结构。作为一种禁带宽度高达6.0eV左右的超宽禁带半导体材料，六方氮化硼(hBN)具有许多优异的特性，例如，优异的物理和化学稳定性、高热导率、高介电强度等，使得近年来其潜在的应用价值被广泛关注与研究。
掺杂是改变半导体材料电学性质的重要手段，也是半导体材料能否实现器件应用的关键。但宽禁带III族氮化物半导体材料的高效P型掺杂是公认的技术难题，因此，寻求合适的掺杂方法与掺杂剂以制备P型的hBN材料具有重要研究意义。
Ⅳ族元素C在Ⅲ-Ⅴ族半导体材料hBN中是一种两性杂质，其电学行为取决于C原子在hBN晶体中的状态，当其替位hBN晶体中的N原子时，可作为受主杂质电离出空穴，因而，利用C掺杂制备P型hBN薄膜是可能的。相比于离子注入、扩散等后掺杂工艺，原位掺杂技术具有工艺简单、杂质分布均匀、不损伤晶格等优点，是调控外延层电学性质的重要手段。
目前，有关C掺杂hBN的研究相对较少，除了非故意C掺杂的研究之外，主要研究都集中在以甲烷(CH4)为掺杂剂的N型掺杂研究上。例如，美国德州理工大学的H.X.Jiang教授团队(Uddin,M.R.,Li,J.,Lin,J.Y.&Jiang,H.X.Probing carbon impurities inhexagonal boron nitride epilayers.Applied Physics Letters 110,doi:10.1063/1.4982647(2017))以甲烷为掺杂源，使用MOCVD制备了C掺杂的N型hBN薄膜，其样品的杂质电离能为0.45eV。使用其他C源以及P型掺杂的研究均未有报导。
发明内容
本发明的目的在于提供一种稳定、高效、简单的原位C掺杂的P型六方氮化硼薄膜及其制备方法。本发明是采用低压化学气相沉积(LPCVD)技术，以三氯化硼(BCl3)、氨气(NH3)为前驱体，二茂镁(Cp2Mg)为掺杂气体制备原位C掺杂的P型六方氮化硼薄膜。
本发明所述的一种原位C掺杂的P型hBN薄膜的制备方法，其步骤如下：
(1)将衬底(包括但不限于硅片、蓝宝石等)依次使用丙酮、乙醇、去离子水分别超声清洗3～8min，然后放入LPCVD设备的腔室；
(2)将腔室真空度抽至5×10-4Pa以下，向腔室中通入高纯氮气使腔室气压稳定在50～500Pa后，对腔室进行升温；
(3)本征hBN薄膜缓冲层的生长：腔室升温至700～900℃后，使用N2作为载气，分别携带BCl3与NH3进入腔室进行缓冲层生长，其中BCl3流量为1～10sccm，NH3流量为1～100sccm；反应原理为：BCl3+NH3→hBN+HCl，缓冲层生长的时间为1～5min，得到厚度为50～250nm的本征hBN薄膜缓冲层；
(4)C掺杂P型hBN薄膜的生长：关闭步骤(3)的所有反应源，将腔室继续升温至1000～1400℃，然后再次开启BCl3与NH3，使用N2作为载气，BCl3流量为10～100sccm，NH3流量为10～1000sccm；同时将Cp2Mg以25～50℃水浴加热挥发，并使用N2作为载气经稀释后携带汇入BCl3的管路中；汇入时可采用连续汇入或脉冲汇入两种方式，采用连续汇入时，Cp2Mg汇入的流量为5～25μmol/min，采用脉冲汇入时，脉冲周期为2～20s，占空比为1/4～3/4；本步骤生长时间为0.5～5h，可在本征hBN薄膜缓冲层上制备得到厚度为0.5～5μm的C掺杂P型hBN薄膜；
(5)关闭步骤(4)的所有反应源结束生长；在氮气的保护下，先以8～15℃/min的降温速率将腔室进行受控降温至380～420℃，以保证高温状态下生长的薄膜样品与腔室不因温度梯度过大而破坏，之后再使腔室自然降温至室温；
(6)将步骤(5)降至室温的腔室充入氮气，使腔室气压回到常压；打开腔室，取出薄膜样品，从而在衬底上完成C掺杂P型hBN薄膜的制备。
本发明的优点在于：
(1)工艺简单且稳定，制备成本低廉，有望应用于大规模生产；
(2)通过对反应源流量与比例、反应温度、气压、掺杂源水浴加热温度与稀释程度等工艺参数的调整，能够精准把控样品的质量、厚度、掺杂浓度、导电性等关键性能指标；
(3)原位掺杂的浓度均匀，且不需要杂质激活，能够制备出空穴浓度较高的P型hBN薄膜；
(4)通过异质外延等方式，可以与其他半导体材料形成各种半导体器件，应用前景广泛。
附图说明
图1：本发明使用的定制卧式LPCVD设备腔室结构示意图。如图1所示，在石英管反应腔室内设有石墨加热台，石英管外侧绕有电磁感应加热线圈作为加热系统，衬底放置在石墨加热台上进行加热。石英管反应腔室分别设有两进气口提供反应前驱体与掺杂源，本发明中，NH3使用一进气口通入，BCl3与Cp2Mg汇合后使用另一进气口通入；
图2：本发明实施例1制备的原位C掺杂P型hBN薄膜的XRD图谱；
图3：本发明实施例1制备的原位C掺杂P型hBN薄膜的EDS能谱；
图4：本发明实施例1制备的原位C掺杂P型hBN薄膜的I-V特性曲线；
图5：本发明实施例1制备的原位C掺杂P型hBN薄膜的杂质电离能拟合曲线。
具体实施方式
实施例1：
(1)将蓝宝石衬底依次使用丙酮、乙醇、去离子水分别超声清洗5min后，然后放入LPCVD设备的腔室；
(2)将设备腔室真空度抽至5×10-4Pa以下。向腔室中通入高纯氮气使腔室气压稳定在100Pa后，使用电磁感应加热系统对腔室进行升温；
(3)本征hBN薄膜缓冲层的生长：腔室升温至700℃后，使用N2作为载气，分别携带BCl3与NH3进入腔室进行反应，其中BCl3流量为10sccm，NH3流量为30sccm。反应原理为：BCl3+NH3→hBN+HCl，缓冲层生长的时间为3min，得到厚度为150nm的本征hBN薄膜缓冲层；
(4)C掺杂P型hBN薄膜的生长：关闭反应源并将腔室继续升温至1200℃后，再次开启BCl3与NH3，使用N2作为载气，使BCl3流量为20sccm，NH3流量为60sccm。同时将Cp2Mg以40℃水浴加热挥发，并使用N2为载气经稀释后携带汇入BCl3的管路中，汇入时采用连续汇入方式，汇入Cp2Mg的流量为18μmol/min。本步骤生长时间为2h，可在缓冲层上制备得到的厚度为2μm的C掺杂P型hBN薄膜；
(5)关闭步骤(4)中的所有反应源，结束生长。在氮气的保护下，先以10℃/min的降温速率对腔室进行受控降温至400℃，以保证高温状态下生长的样品与腔室不因温度梯度过大而破坏，之后使腔室自然降温至室温；
(6)腔室降温至室温后，充入氮气使腔室气压回到常压，打开腔室，取出薄膜样品，从而在衬底上完成C掺杂P型hBN薄膜的制备。
对上述薄膜进行XRD表征的结果如图2所示，薄膜的衍射峰位于25.95°，对应hBN(002)晶面的衍射峰；其半峰宽为1.163°，证明薄膜质量良好。
图3为薄膜的EDS能谱，从中可以明显观察到B、N、C、O四个元素的Kα特征峰，证明C元素成功被掺入hBN薄膜中。此外，未见到Mg元素的特征峰，表明没有将Mg掺入薄膜中。
对C掺杂hBN薄膜进行室温下的I-V特性测试，并使用本征hBN薄膜在相同条件下测试以进行对比，其结果如图4所示。为了方便与本征hBN薄膜的I-V特性相比较，图4采用的是半对数坐标。图4中的插图是掺杂薄膜在线性坐标系下的I-V特性。在100V偏压下，流过C掺杂hBN薄膜的电流可达4×10-4A，导电性相较于本征材料(～10-10A@100V)得到大幅提升。由插图可以看到，C掺杂hBN薄膜的I-V特性接近线性，证明薄膜与电极之间能够形成良好的欧姆接触。
通过变温I-V测试对薄膜进行了杂质电离能拟合，其结果如图5所示。拟合所得的杂质电离能为321meV。
对薄膜进行霍尔效应测试得到的结果为：霍尔系数RH＝992cm3/C＞0，表明薄膜为P型导电，电阻率约为880Ω·cm，空穴浓度约为2.01×1015cm-3，霍尔迁移率为3.55cm2/(V·s)，电学特性良好。
实施例2：
(1)将蓝宝石衬底依次使用丙酮、乙醇、去离子水分别超声清洗5min后，然后放入LPCVD设备的腔室；
(2)将设备腔室真空度抽至5×10-4Pa以下。向腔室中通入高纯氮气使腔室气压稳定在100Pa后，使用电磁感应加热系统对腔室进行升温；
(3)本征hBN薄膜缓冲层的生长：腔室升温至700℃后，使用N2作为载气，分别携带BCl3与NH3进入腔室进行反应，其中BCl3流量为10sccm，NH3流量为30sccm。反应原理为：BCl3+NH3→hBN+HCl，缓冲层生长的时间为2min，可得到厚度为100nm的缓冲层；
(4)C掺杂P型hBN薄膜的生长：关闭反应源并将腔室继续升温至1200℃后，再次开启BCl3与NH3，使用N2作为载气，使BCl3流量为20sccm，NH3流量为60sccm。同时将Cp2Mg以40℃水浴加热挥发，并使用N2为载气经稀释后携带汇入BCl3的管路中，汇入时采用脉冲汇入方式，脉冲周期为10s，占空比为1/2。本步骤生长时间为2h，可在缓冲层上制备得到的厚度为2μm的C掺杂P型hBN薄膜；
(5)关闭步骤(4)中的所有反应源，结束生长。在氮气的保护下，先以10℃/min的降温速率对腔室进行受控降温至400℃，以保证高温状态下生长的样品与腔室不因温度梯度过大而破坏，之后使腔室自然降温至室温；
(6)腔室降温至室温后，充入氮气使腔室气压回到常压，打开腔室，取出薄膜样品，从而在衬底上完成C掺杂P型hBN薄膜的制备。
对薄膜进行霍尔效应测试得到的结果为：霍尔系数RH＝1.28×103cm3/C＞0，表明薄膜为P型导电，电阻率约为2196Ω·cm，空穴浓度约为1.63×1015cm-3，霍尔迁移率为1.74cm2/(V·s)，电学特性良好。
Claims (8)
1.一种原位C掺杂的P型hBN薄膜的制备方法，其步骤如下：
(1)将衬底依次使用丙酮、乙醇、去离子水分别超声清洗3～8min，然后放入低压化学气相沉积设备的腔室；
(2)将腔室真空度抽至5×10-4Pa以下，向腔室中通入高纯氮气使腔室气压稳定在50～500Pa后，对腔室进行升温；
(3)本征hBN薄膜缓冲层的生长：腔室升温至700～900℃后，使用N2作为载气，分别携带BCl3与NH3进入腔室进行缓冲层生长，得到厚度为50～250nm的本征hBN薄膜缓冲层；
(4)C掺杂P型hBN薄膜的生长：关闭步骤(3)的所有反应源，将腔室继续升温至1000～1400℃，然后再次开启BCl3与NH3，使用N2作为载气；同时将Cp2Mg以25～50℃水浴加热挥发，并使用N2作为载气经稀释后携带汇入BCl3的管路中，在本征hBN薄膜缓冲层上制备得到厚度为0.5～5μm的C掺杂P型hBN薄膜；
(5)关闭步骤(4)的所有反应源结束生长；在氮气的保护下，将腔室进行受控降温至380～420℃，之后再使腔室自然降温至室温；
(6)将步骤(5)降至室温的腔室充入氮气，使腔室气压回到常压；打开腔室，取出薄膜样品，从而在衬底上完成C掺杂P型hBN薄膜的制备。
2.如权利要求1所述的一种原位C掺杂的P型hBN薄膜的制备方法，其特征在于：步骤(1)中的衬底为硅片或蓝宝石。
3.如权利要求1所述的一种原位C掺杂的P型hBN薄膜的制备方法，其特征在于：步骤(3)中，BCl3流量为1～10sccm，NH3流量为1～100sccm，生长时间为1～5min。
4.如权利要求1所述的一种原位C掺杂的P型hBN薄膜的制备方法，其特征在于：步骤(4)中BCl3流量为10～100sccm，NH3流量为10～1000sccm，生长时间为0.5～5h。
5.如权利要求1所述的一种原位C掺杂的P型hBN薄膜的制备方法，其特征在于：步骤(4)中Cp2Mg采用连续汇入或脉冲汇入两种方式汇入BCl3的管路。
6.如权利要求5所述的一种原位C掺杂的P型hBN薄膜的制备方法，其特征在于：采用连续汇入时，Cp2Mg汇入的流量为5～25μmol/min；采用脉冲汇入时，脉冲周期为2～20s，占空比为1/4～3/4。
7.如权利要求1所述的一种原位C掺杂的P型hBN薄膜的制备方法，其特征在于：步骤(5)的降温速率为8～15℃/min。
8.一种原位C掺杂的P型hBN薄膜，其特征在于：是由权利要求1～7任何一项所述的方法制备得到。
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