CN114907360A - 一种无金属铁电纳米晶mdabco-nh4i3的制备方法 - Google Patents
一种无金属铁电纳米晶mdabco-nh4i3的制备方法 Download PDFInfo
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Abstract
本发明涉及一种宽带隙无金属钙钛矿铁电纳米晶MDABCO‑NH4I3的制备方法，包括如下步骤：(1)将NH4I(固体溶解在N，N‑二甲基甲酰胺和HI酸的混合溶液中，再向其中加入一定量的油酸和正辛胺；(2)将MDABCOI固体单独溶解在N，N‑二甲基甲酰胺中，再加入到上述前驱体溶液中，充分反应，加入乙酸乙酯，迅速产生白色固体；(3)用乙酸乙酯洗涤离心，40℃干燥，得到成品。本发明利用长链的油酸和正辛胺，在室温条件下有效控制NH4I与MDABCOI的反应过程，通过有效调节两者比例，制备出纯相结构的无金属钙钛矿纳米晶MDABCO‑NH4I3。这种方法具有反应时间短、设备简单、成本低等优点，是一种全新的制备宽带隙无金属钙钛矿铁电纳米晶MDABCO‑NH4I3的方法。
Description
技术领域
本发明涉及压电材料领域，具体涉及一种光/压电催化剂无金属钙钛矿纳米晶MDABCO-NH4I3的制备方法。
背景技术
传统能源的枯竭问题和环境问题日益严重。而压电材料可以将环境中的一次能源(如机械能)转换为二次能源(如化学能)，为获取可再生能源提供了良好的范例。
卤化钙钛矿因其结构简单、光吸收强、载流子迁移率高等优点，已被广泛应用于太阳能电池、发光二极管等领域。卤化钙钛矿材料在催化领域的研究则刚刚起步。然而，传统的窄带隙钙钛矿材料由于阳离子的毒性仍然会引起环境问题，很难实现大规模的商用。无金属钙钛矿铁电材料是一类新型宽带隙的钙钛矿材料，显示出有吸引力的铁电和压电特性。由于其铁电/压电性，可以与常见的光催化进行联动，大大拓宽其在催化领域的应用。
无金属铁电钙钛矿单晶制备已有所报道，铁电单晶材料主要应用于非线性激光器等。本发明首次实现了纳米结构的无金属钙钛矿铁电纳米晶MDABCO-NH4I3的制备，由于不含金属、常温制备以及纳米结构等特质，在光/压电催化等领域具有很好的应用前景。
据申请人所知，无金属钙钛矿铁电纳米晶MDABCO-NH4I3的制备还没被报道过，是一种全新的合成方法。
发明内容
本发明的目的是制备无金属钙钛矿铁电MDABCO-NH4I3纳米晶，可以避免重金属毒性、成本昂贵等问题。
本发明的具体技术方案如下：
一种无金属钙钛矿铁电纳米晶MDABCO-NH4I3的制备方法，包括如下步骤：
(1)将10mL DMF和2.5mL氢碘酸加入到圆底三颈烧瓶中，再加入1mL磷酸防止碘离子氧化，溶解后，称取5mmol，0.72g NH4I固体，充分溶解后，将1mL油酸和0.5mL正辛胺加入到上述混合液中，搅拌2h；
(2)MDABCOI(典化N，N-二氨基-1，4-二氮杂二环[2.2.2]辛烷)的制备：将2g，0.0178mol DABCO(1，4-二氮杂二环[2.2.2]辛烷)加入到三颈烧瓶中，加入到50mL正己烷中使其完全溶解，然后向溶液中缓慢加入1.11mL碘甲烷(0.0178mol)，继续反应1.5h，反应完全后，将白色沉淀在离心速度为12000rpm条件下离心5min，用正己烷反复洗涤3-5次后，样品于40℃下烘干，密封保存以备后用；
(3)称取1.5mmol MDABCOI固体单独溶解在DMF中后，快速加入到(1)溶液中，继续搅拌5min；
(4)加入20mL乙酸乙酯，迅速形成白色乳浊液，收集沉淀于12000rpm高速离心机中离心，反复洗涤5-7次后，干燥备用。
NH4I和MDABCOI的摩尔比对于得到纯相结构的无金属钙钛矿铁电MDABCO-NH4I3纳米晶至关重要，当两者摩尔比大于等于10∶2且小于等于10∶3时，能够得到有纯的钙钛矿相。而如果采用化学剂量比的1∶1，则得不到纯相结构的MDABCO-NH4I3。
步骤(3)中，所述MDABCOI加入前驱体后的反应时间为5min，较短的反应时间可以抑制单晶的成核，从而形成较小的纳米尺寸。
步骤(3)中，所述洗涤溶液为乙酸乙酯。
本发明在室温条件下有效控制NH4I与MDABCOI的反应过程，第一次制备出纳米量级纯相结构的无金属钙钛矿铁电纳米晶MDABCO-NH4I3。这种方法具有反应时间短、操作简单等优点，是一种全新的制备无金属全有机铁电MDABCO-NH4I3纳米晶的方法。
附图说明
图1无金属钙钛矿铁电材料MDABCO-NH4I3的化学结构；
图2为实施例1制备的MDABCO-NH4I3成品的XRD图谱；
图3为实施例1中所获得的成品的SEM图及元素分析能谱图；
图4为实施例1中所获得的成品的TEM图谱；
图5为实施例1中所获得的成品的紫外可见吸收谱；
图6为实施例1中所获得的成品的(a)热重曲线，(b)差热分析DSC图。
图7MDABCO-NH4I3纳米晶压电催化降解苏丹红(III)吸收光谱
具体实施方式
实施例1
向100mL单颈烧瓶中加入10mL N，N-二甲基甲酰胺和2.5mL盐酸，称取5mmol NH4I固体，搅拌使之完全溶解，再向其中加入1mL油酸和0.5mL正辛胺，搅拌2h。然后称取1.5mmolMDABCOI固体单独溶解在N，N-二甲基甲酰胺中后逐滴加入到前驱体溶液中，继续搅拌5min，向其中加入20mL乙酸乙酯，迅速产生白色沉淀，将溶液在12000r/min高速离心机中洗涤离心5-7次，将洗涤离心后固体于40℃下干燥12小时，得到MDABCO-NH4I3成品。
实施例2
图1无金属钙钛矿铁电材料MDABCO-NH4I3的结构和化学结构。图2是各种比例的前驱体材料合成的纳米晶的XRD图。与报道的MDABCO-NH4I3单晶衍射峰对比，当前驱体NH4I与MDABCOI摩尔比大于10∶3时，衍射峰在20.1°、23.8°以及25.84°出现轻微的杂峰(图中星号代表杂相)。当前驱体摩尔比小于等于10∶3并大于等于10∶2时，晶型与单晶纯相一致。结果表明，制备出纯相的MDABCO-NH4I3纳米晶。
实施例3
为了进一步表征其尺寸大小和形貌，我们对MDABCO-NH4I3样品进行了SEM、EDS和TEM的表征。图3为低倍率下MDABCO-NH4I3纳米晶的SEM图像，可以明显看出纳米晶的形状和均匀性，表明制备的纳米晶几乎是单分散的。在中等放大率下该图像清楚地显示了尺寸在370-650nm之间的均匀纳米立方体。此外，从SEM图像中未观察到团聚或其他结构，表明成功制备了这一新型纳米尺寸的纯有机无金属卤化钙钛矿材料。SEM-EDS结果表明了纳米晶的表面形貌，证实了钙钛矿结构中存在C、N和I元素，N与I的元素比为1∶1。TEM图像(图4)进一步证实了MDABCO-NH4I3纳米立方体的形成。
实施例4
如图5，通过紫外可见吸收分别对上述实施例1制得的MDABCO-NH4I3纳米晶溶液的光学吸收和发光特性进行了分析。根据公式(αhv)n＝A(hv-Eg)，其中α，h，v，Eg和A分别是吸光系数、普朗克常量、光子频率、半导体禁带宽度和常数，n值取决于半导体的带间跃迁类型，即直接带隙还是间接带隙。我们将MDABCO-NH4I3样品的吸收光谱曲线拟合成(αhv)2与hv之间的关系曲线(图4插图)，发现MDABCO-NH4I3样品的带隙为5.63eV，是一种有别于常见窄带隙钙钛矿材料的宽带隙钙钛矿铁电材料。
实施例5
图6(a)为MDABCO-NH4I3纳米晶重量随温度的变化曲线。分析表明热分解温度约为517.9K。由图6(b)的差热分析可知，升温曲线在431K附近的峰表明发生了铁电-顺电的相变，而在降温曲线中在372K附近的峰是因为发生了顺电-铁电的相变。这个相变温度高于绝大多数高温分子铁电体和典型的铁电体BaTiO3(393K)，表明这个材料可以在室温到较高温度下(431K)保持铁电/压电性能，具有很好的应用前景。
实施例6
将MDABCO-NH4I3纳米晶分散至的苏丹红(III)溶液中。室温下在100W超声环境下开始压电催化过程。通过紫外分光光度计在特征波长处分析剩余苏丹红(III)浓度的变化。图7为纳米晶压电光催化降解苏丹红(III)的紫外吸收图，通过紫外吸收的下降表明纳米晶有明显的压电催化降解有机物效果。
本发明不限于上述实施方式，任何采用与本结构相同或相似的制备方法，均在本发明的保护范围内。
Claims (5)
1.一种无金属钙钛矿铁电纳米晶MDABCO-NH4I3的制备方法，其特征在于包含如下步骤：
(1)将NH4I固体溶解在N，N-二甲基甲酰胺和HI酸的混合溶液中，向其中加入一定量的油酸和正辛胺，搅拌反应使之完全溶解；
(2)通过DABCO与碘甲烷在正己烷中反应制备MDABCOI；
(3)将MDABCOI固体加入到上述前驱体溶液中，继续搅拌反应5分钟，加入乙酸乙酯，迅速产生白色固体；
(4)用乙酸乙酯洗涤，在12000r/min高速离心机中离心，干燥，得到成品。
2.根据权利要求1所述的方法，其特征在于步骤(1)中，所述N，N-二甲基甲酰胺和HI酸的混合溶液中两者体积比为4∶1。
3.根据权利要求1所述的方法，其特征在于步骤(1)中，所述油酸和正辛胺的体积比为2∶1。
4.根据权利要求1所述的方法，其特征在于步骤(3)中，所述NH4I和MDABCOI的摩尔比为大于等于10∶2且小于等于10∶3。
5.根据权利要求1所述的方法，其特征在于步骤(4)中，所述洗涤溶液为乙酸乙酯。
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| HENG-YUN YE ET AL.: "Metal-free three-dimensional perovskite ferroelectrics" * |
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| CN115445656A (zh) * | 2022-09-26 | 2022-12-09 | 南京工业大学 | 钙钛矿型光/压电共催化剂(4-氨基四氢吡喃)2PbBr4纳米晶的制备与应用 |
| CN115445656B (zh) * | 2022-09-26 | 2023-12-19 | 南京工业大学 | 钙钛矿型光/压电共催化剂(4-氨基四氢吡喃)2PbBr4纳米晶的制备与应用 |
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