CN112234110A - 一种三明治状pn结及其精准构筑方法 - Google Patents
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Abstract
本发明属于PN结技术领域，本发明提供了一种三明治状PN结，所述的三明治状PN结是在三层晶胞厚度半导体材料中构筑的。本发明还提供了一种三明治状PN结的精准构筑方法。本发明的三明治状PN结均匀整齐，有透明感，尺寸在微米级；本发明的三明治状PN结厚度与三层晶胞半导体材料的厚度完全吻合；本发明的构筑方法具有精确可控性，广泛适用于各种半导体材料，对于发挥材料本身性质并进一步提高光电化学性能具有重大意义。
Description
技术领域
本发明涉及PN结技术领域,尤其涉及一种三明治状PN结及其精准构筑方法。
背景技术
利用太阳光将水转化为氢和氧的光电化学(PEC)水分解法，是一种实现可再生能源转化和存储的前景光明的方法。为了实现有效的光电能量转换，至关重要的是设计和制造理想的半导体光电极，以提高可见光的收集率和光激载流子的分离/转移效率，加速析氧动力学。最近，由于具有独特的光电特性，二维(2D)类石墨烯层状材料已发展成为有前途的PEC电极。但是，严重的电荷重组和缓慢的氧释放反应(OER)动力学严重阻碍了二维层状半导体材料的PEC性能。
调控尺寸和形态，掺杂和构建PN结是解决上述问题的有效策略。在各种形态材料中，三明治状结构的材料，可以提高太阳光的利用率，缩短电荷载流子的扩散长度，为目标反应物的吸附提供巨大的表面积并暴露出足够多的活性位点以进行表面反应。由于这种结构是由多种不同的半导体构成，因此，理想的异质结的实现不仅取决于其能带排列，而且还受其晶体结构、晶格参数等其它特征的影响，这使其难以在实际应用中实现。但是，单一材料中的同质结在上述方面明显具有优势。此外，这种同质结的连续带弯曲对于载流子分离和电荷转移非常有利。
以n型半导体为例，研究者们已广泛尝试了一系列受体掺杂剂以引入P型特性，从而建立PN同质结。尽管取得了一些进展，但是由于缺乏可行的策略和合适的模型，在单个原子级别的2D材料中实现三明治状PN同质结仍然面临着巨大的挑战。因此，进一步探索PN同质结将深化对半导体物理学的理解并推动相关新技术的发展。
发明内容
本发明的目的在于为了克服现有技术的不足而提供一种三明治状PN结及其精准构筑方法。本发明的三明治状PN结均匀整齐，有透明感，尺寸在微米级；本发明的三明治状PN结厚度与三层晶胞半导体材料的厚度完全吻合；本发明的构筑方法具有精确可控性，广泛适用于各种半导体材料。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种三明治状PN结，所述的三明治状PN结是在三层晶胞厚度半导体材料中构筑的。
作为优选，所述的半导体材料为ZnIn2S4或双元素半导体材料。
作为优选，所述的双元素半导体材料为SnS2、TiO2、In2O3、ZnO、Fe2O3、MoS2、ZnS或CdS。
本发明还提供了一种三明治状PN结的精准构筑方法，包括如下步骤：
1)将锡盐、硫源、含铵根离子的物质与溶剂混合，得到反应液；
2)将反应液与掺杂氟的SnO2导电玻璃混合后进行反应，得到三层晶胞厚度二硫化锡纳米片阵列；
3)将含第五主族元素的物质与三层晶胞厚度二硫化锡纳米片阵列在惰性气氛下进行反应，得到三明治状PN结。
作为优选，步骤1)所述锡盐为硫酸锡、草酸锡、氯化锡或锡酸钠，所述硫源为硫脲、硫代乙酰胺或硫代硫酸钠，所述含铵根离子的物质为氨水、硫化铵、硫酸铵、四甲基铵或碳酸氢铵，所述溶剂为水、异丙醇、乙二醇或乙醇。
作为优选，步骤2)所述反应的温度为100～200℃，时间为0.5～48h。
作为优选，步骤2)所述混合前掺杂氟的SnO2导电玻璃经过超声清洗，所述掺杂氟的SnO2导电玻璃与反应液的体积比为1:1～10，所述反应完成后在真空条件下进行干燥，所述干燥的温度为50～70℃，所述真空度为0.03～0.07MPa。
作为优选，步骤3)所述反应的温度为200～600℃，时间为1～240min，所述惰性气体的流量为30～100sccm，所述惰性气体为氩气。
作为优选，步骤3)所述含第五主族元素的物质为氨基酸、丙氨酸、氯化铵、氨气、氮气、硝酸铵、碳酸氢铵、红磷、次亚磷酸钠或磷化氢气体。
作为优选，步骤3)升温至反应温度的速率为2～10℃/min，当所述含第五主族元素的物质为气体时，所述气体的流量为总流量的1～30％。
本发明的有益效果包括以下几点：
1)本发明的三明治状PN结均匀整齐，有透明感，尺寸在微米级。
2)本发明的三明治状PN结具有精确可控性，对于发挥材料本身性质并进一步提高光电化学性能具有重大意义。
附图说明
图1为实施例3的三明治状PN结的XRD图，其中，FTO为导电玻璃的XRD图；
图2为实施例3的三明治状PN结的SEM图；
图3为实施例3的三明治状PN结的TEM及HRTEM图；
图4为实施例3的三明治状PN结的AFM图；
图5为实施例3的三明治状PN结的EDS mapping图；
图6为实施例3的三明治状PN结的莫特肖特基曲线；
图7为实施例3的三明治状PN结的原子模型；
图8为实施例3的三明治状PN结的示意图；
图9为实施例4的三明治状PN结的XRD图；
图10为实施例5的三明治状PN结的XRD图；
图11为实施例6的三明治状PN结的XRD图；
图12为实施例7的三明治状PN结的XRD图；
图13为实施例8的三明治状PN结的XRD图；
图14为实施例9的三明治状PN结的XRD图；
图15为实施例10的三明治状PN结的XRD图；
图16为实施例11的三明治状PN结的XRD图。
具体实施方式
本发明提供了一种三明治状PN结，所述的三明治状PN结是在三层晶胞厚度半导体材料中构筑的。
本发明所述的半导体材料优选为ZnIn2S4或双元素半导体材料，所述的双元素半导体材料优选为SnS2、TiO2、In2O3、ZnO、Fe2O3、MoS2、ZnS或CdS。
本发明还提供了一种三明治状PN结的精准构筑方法，包括如下步骤：
1)将锡盐、硫源、含铵根离子的物质与溶剂混合，得到反应液；
2)将反应液与掺杂氟的SnO2导电玻璃混合后进行反应，得到三层晶胞厚度二硫化锡纳米片阵列；
3)将含第五主族元素的物质与三层晶胞厚度二硫化锡纳米片阵列在惰性气氛下进行反应，得到三明治状PN结。
本发明步骤1)所述锡盐优选为硫酸锡、草酸锡、氯化锡或锡酸钠，所述硫源优选为硫脲、硫代乙酰胺或硫代硫酸钠，所述锡盐中锡元素的摩尔量与硫源中硫元素的摩尔量之比优选为1:2；所述含铵根离子的物质优选为氨水、硫化铵、硫酸铵、四甲基铵或碳酸氢铵，所述含铵根离子的物质优选为0.05～20mmol，进一步优选为0.1～10mmol；所述溶剂优选为水、异丙醇、乙二醇或乙醇，所述溶剂的量优选能够充分溶解锡盐、硫源。
本发明所述的含铵根离子的物质通过提供铵根离子，对纳米片的厚度进行调控。
本发明步骤2)所述反应的温度优选为100～200℃，进一步优选为120～180℃，更优选为140～160℃；所述反应的时间优选为0.5～48h，进一步优选为5～24h，更优选为10～20h。
本发明步骤2)所述混合前掺杂氟的SnO2导电玻璃优选经过超声清洗，所述超声清洗的溶剂优选为丙酮、乙醇、去离子水、异丙酮、洗洁精、专业导电玻璃清洗液、浓H2SO4、H2O2和氢氟酸中的一种或几种，进一步优选为丙酮、乙醇和去离子水；所述超声清洗的时间优选为30～100min，进一步优选为50～90min；所述导电玻璃清洗后优选进行干燥处理。
本发明根据掺杂氟的SnO2导电玻璃上污垢的量选择合适的清洗方式和超声时间，为了保证清洗的干净度，可以适当延长超声时间。
本发明步骤2)所述掺杂氟的SnO2导电玻璃与反应液的体积比优选为1:1～10，进一步优选为1:3～7。
本发明步骤2)所述混合优选将干燥的导电玻璃放入聚四氟乙烯内胆后缓慢将反应液滴入内胆中，所述反应液优选不完全浸没导电玻璃。
本发明步骤2)所述反应完成后，优选自然降温至室温；所述掺杂氟的SnO2导电玻璃优选在真空条件下进行干燥，所述干燥的温度优选为50～70℃，进一步优选为60～65℃，所述真空度优选为0.03～0.07MPa，进一步优选为0.04～0.06MPa。
本发明步骤2)对掺杂氟的SnO2导电玻璃在真空条件下进行干燥的目的是降低氧含量，防止氧化。
本发明步骤3)所述反应的温度优选为200～600℃，进一步优选为300～500℃，更优选为400℃；所述反应的时间优选为1～240min，进一步优选为10～200min，更优选为100～150min；所述惰性气体的流量优选为30～100sccm，进一步优选为50～90sccm，更优选为60～80sccm；所述惰性气体优选为氩气。
本发明步骤3)所述含第五主族元素的物质优选为氨基酸、丙氨酸、氯化铵、氨气、氮气、硝酸铵、碳酸氢铵、红磷、次亚磷酸钠或磷化氢气体，进一步优选为氨基酸、氯化铵或氨气。
本发明步骤3)升温至反应温度的速率优选为2～10℃/min，进一步优选为4～8℃/min，更优选为5～7℃/min；所述升温的起始温度优选为20℃；所述反应优选在密封环境下进行，所述反应前优选通入惰性气体排空空气。
本发明步骤3)所述含第五主族元素的物质与三层晶胞厚度的二硫化锡纳米片阵列的摩尔比优选为5～200：1，进一步优选为20～150：1，更优选为50～100：1。
本发明步骤3)所述含第五主族元素的物质为气体时，所述气体的流量优选为总流量的1～30％，进一步优选为5～20％，更优选为10～15％；所述气体通入时间优选和反应时间相同。
本发明所述总流量为含第五主族元素的气体和惰性气体的总流量，惰性气体起到载气的作用，目的是控制含第五主族元素气体的比例。
本发明所述含第五主族元素的物质与三层晶胞厚度二硫化锡纳米片阵列反应的原理为含第五主族元素的物质气化或分解为含有第五主族元素的气体，气体在高温环境下化学键断裂后生成第五主族元素，第五主族元素再与三层晶胞厚度二硫化锡纳米片结合，占据晶格。
本发明的二硫化锡(SnS2)是一种可见光响应、结构稳定、活性较好的半导体材料，由于存在少量固有的硫空位，而使得材料呈现N型导电性，可作为研究三层晶胞厚度PN结的良好模型，并通过在最外两层精确引入受体掺杂原子，构成了P-N-P型的三明治状PN结。本发明的构筑方法得到的三明治状PN结均匀整齐，有透明感，尺寸在微米级；三明治状PN结厚度为1.79nm且具有3层原子，与三层晶胞SnS2的厚度完全吻合。本发明三明治状PN结的构筑方法得到的氮元素全部掺杂在最外层两个表面，具有精确可控性，本发明的构筑方法广泛适用于各种半导体材料，对于发挥材料本身性质并进一步提高光电化学性能具有重大意义。
下面结合实施例对本发明提供的技术方案进行详细的说明，但是不能把它们理解为对本发明保护范围的限定。
实施例1
将掺杂氟的SnO2导电玻璃(导电玻璃FTO)分别在丙酮、乙醇和去离子水中各连续超声30min，干燥、备用。将硫酸锡和硫脲按原子比Sn:S＝1:2放入烧杯中，加入0.1mmol氨水和适量的去离子水进行充分搅拌，得到反应液。然后，将干燥的导电玻璃FTO放入聚四氟乙烯内胆中，缓慢将反应液滴入内胆中，导电玻璃FTO与反应液的体积比为1:2，反应液不完全浸没导电玻璃。将聚四氟乙烯内胆放入高压反应釜，再将高压反应釜放入烘箱中，在100℃下反应40h。反应完成后，自然降温至室温。打开反应釜，导电玻璃FTO上形成了薄膜，将导电玻璃FTO取出后使用去离子水和乙醇进行反复清洗，然后在真空度为0.03MPa，温度为60℃的真空干燥箱中进行干燥，得到三层晶胞厚度二硫化锡纳米片阵列。
将50g的氨基酸固体与三层晶胞厚度二硫化锡纳米片阵列分别放置在石墨舟的头尾两端，氨基酸固体与三层晶胞厚度二硫化锡纳米片阵列的摩尔比为10：1，再将石墨舟放置在可程序控温的管式炉中，其中，氨基酸固体放置在气流的上游，三层晶胞厚度二硫化锡纳米片阵列放置在中心温区。将管式炉密封后通入流量为30sccm的氩气排空空气，在起始温度为20℃下以2℃/min的升温速率升温至300℃，反应240min后自然降至室温，即得三明治状PN结。
实施例2
将掺杂氟的SnO2导电玻璃(导电玻璃FTO)分别在丙酮、乙醇和去离子水中各连续超声30min，干燥、备用。将氯化锡和硫代乙酰胺按原子比Sn:S＝1:2放入烧杯中，加入10mmol硫酸铵和适量的异丙醇进行充分搅拌，得到反应液。然后，将干燥的导电玻璃FTO放入聚四氟乙烯内胆中，缓慢将反应液滴入内胆中，导电玻璃FTO与反应液的体积比为1:10，反应液不完全浸没导电玻璃。将聚四氟乙烯内胆放入高压反应釜，再将高压反应釜放入烘箱中，在200℃下反应2h。反应完成后，自然降温至室温。打开反应釜，导电玻璃FTO上形成了薄膜，将导电玻璃FTO取出后使用去离子水和乙醇进行反复清洗，然后在真空度为0.07MPa，温度为50℃的真空干燥箱中进行干燥，得到三层晶胞厚度二硫化锡纳米片阵列。
将200g的氯化铵固体与三层晶胞厚度二硫化锡纳米片阵列分别放置在石墨舟的头尾两端，氯化铵固体与三层晶胞厚度二硫化锡纳米片阵列的摩尔比为100：1，再将石墨舟放置在可程序控温的管式炉中，其中，氯化铵固体放置在气流的上游，三层晶胞厚度二硫化锡纳米片阵列放置在中心温区。将管式炉密封后通入流量为100sccm的氩气排空空气，在起始温度为20℃下以10℃/min的升温速率升温至600℃，反应10min后自然降至室温，即得三明治状PN结。
实施例3
将掺杂氟的SnO2导电玻璃(导电玻璃FTO)分别在丙酮、乙醇和去离子水中各连续超声30min，干燥、备用。将草酸锡和硫代硫酸钠按原子比Sn:S＝1:2放入烧杯中，加入5mmol四甲基铵和适量的乙醇进行充分搅拌，得到反应液。然后，将干燥的导电玻璃FTO放入聚四氟乙烯内胆中，缓慢将反应液滴入内胆中，导电玻璃FTO与反应液的体积比为1:6，反应液不完全浸没导电玻璃。将聚四氟乙烯内胆放入高压反应釜，再将高压反应釜放入烘箱中，在150℃下反应20h。反应完成后，自然降温至室温。打开反应釜，导电玻璃FTO上形成了薄膜，将导电玻璃FTO取出后使用去离子水和乙醇进行反复清洗，然后在真空度为0.05MPa，温度为70℃的真空干燥箱中进行干燥，得到三层晶胞厚度二硫化锡纳米片阵列。
将三层晶胞厚度二硫化锡纳米片阵列放置在石墨舟中，再将石墨舟放置在可程序控温的管式炉的中心温区处，将管式炉密封后通入流量为70sccm的氩气排空空气，在起始温度为20℃下以7℃/min的升温速率升温至400℃，当管式炉温度达到400℃时立即通入氨气，氨气与三层晶胞厚度二硫化锡纳米片阵列的摩尔比为50：1，反应100min，保证氨气通入时间和反应时间一致，反应完成后自然降至室温，即得三明治状PN结。
实施例4
将实施例3的SnS2替换为TiO2，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例5
将实施例3的SnS2替换为In2O3，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例6
将实施例3的SnS2替换为ZnO，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例7
将实施例3的SnS2替换为Fe2O3，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例8
将实施例3的SnS2替换为MoS2，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例9
将实施例3的SnS2替换为ZnS，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例10
将实施例3的SnS2替换为CdS，其他步骤与实施例3相同，成功制得三明治状PN结。
实施例11
将实施例3的SnS2替换为ZnIn2S4，其他步骤与实施例3相同，成功制得三明治状PN结。
对实施例3的三明治状PN结进行测试，由图1的XRD图可知，三明治状PN结的SnS2(PNP-SnS2)晶相与纯相的SnS2一致，无杂质生成；由图2的SEM图可知，三明治状PN结生长均匀整齐，且尺寸在微米级，有透明感，说明材料很薄。
由图3的HRTEM图可知，三明治状PN结厚度约为1.8nm且具有3层原子，与三层晶胞SnS2的厚度完全吻合；由图4的AFM图可知，三明治状PN结的厚度为1.79nm，与三层SnS2的厚度一致；由图5的EDS mapping数据可知，氮元素成功掺入材料中，并且精确可控地掺杂在最外层两个表面，证明本专利构筑方法的精确可控性；由图6的莫特肖特基曲线图可知，三明治状PN结的P型和N型共存，本专利的方法成功构筑了三明治状PN结。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种三明治状PN结，其特征在于，所述的三明治状PN结是在三层晶胞厚度半导体材料中构筑的。
2.根据权利要求1所述的三明治状PN结，其特征在于，所述的半导体材料为ZnIn2S4或双元素半导体材料。
3.根据权利要求1或2所述的三明治状PN结，其特征在于，所述的双元素半导体材料为SnS2、TiO2、In2O3、ZnO、Fe2O3、MoS2、ZnS或CdS。
4.权利要求1～3任意一项所述的三明治状PN结的精准构筑方法，其特征在于，包括如下步骤：
1)将锡盐、硫源、含铵根离子的物质与溶剂混合，得到反应液；
2)将反应液与掺杂氟的SnO2导电玻璃混合后进行反应，得到三层晶胞厚度二硫化锡纳米片阵列；
3)将含第五主族元素的物质与三层晶胞厚度二硫化锡纳米片阵列在惰性气氛下进行反应，得到三明治状PN结。
5.根据权利要求4所述的构筑方法，其特征在于，步骤1)所述锡盐为硫酸锡、草酸锡、氯化锡或锡酸钠，所述硫源为硫脲、硫代乙酰胺或硫代硫酸钠，所述含铵根离子的物质为氨水、硫化铵、硫酸铵、四甲基铵或碳酸氢铵，所述溶剂为水、异丙醇、乙二醇或乙醇。
6.根据权利要求5所述的构筑方法，其特征在于，步骤2)所述反应的温度为100～200℃，时间为0.5～48h。
7.根据权利要求6所述的构筑方法，其特征在于，步骤2)所述混合前掺杂氟的SnO2导电玻璃经过超声清洗，所述掺杂氟的SnO2导电玻璃与反应液的体积比为1:1～10，所述反应完成后在真空条件下进行干燥，所述干燥的温度为50～70℃，所述真空度为0.03～0.07MPa。
8.根据权利要求6或7所述的构筑方法，其特征在于，步骤3)所述反应的温度为200～600℃，时间为1～240min，所述惰性气体的流量为30～100sccm，所述惰性气体为氩气。
9.根据权利要求8所述的构筑方法，其特征在于，步骤3)所述含第五主族元素的物质为氨基酸、丙氨酸、氯化铵、氨气、氮气、硝酸铵、碳酸氢铵、红磷、次亚磷酸钠或磷化氢气体。
10.根据权利要求9所述的构筑方法，其特征在于，步骤3)升温至反应温度的速率为2～10℃/min，当所述含第五主族元素的物质为气体时，所述气体的流量为总流量的1～30％。
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