CN113416218A - 一种稀土-镍混金属分子基磁性材料合成方法和应用 - Google Patents
一种稀土-镍混金属分子基磁性材料合成方法和应用 Download PDFInfo
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Abstract
一种稀土‑镍混金属分子基磁性材料及其合成方法和应用,将Gd(hfac)3·2H2O、Tb(hfac)3·2H2O或者Dy(hfac)3·2H2O中的一种或其混合和Ni(hfac)2的混合物加入到正己烷溶液中,加热回流降温后,滴加含有NIT‑4py自由基配体的有机溶液,最后加热搅拌反应一段时间后冷却至室温,静置得到方块状晶体。该稀土‑镍混金属分子基磁性材料在高密度信息存储、量子计算等领域具有巨大的潜在应用价值。
Description
技术领域
本发明属于金属配合物领域,具体涉及一种稀土-镍混金属分子基磁性材料及其合成方法和应用。
背景技术
分子基磁性材料是二十世纪八十年代末发展起来的一种新型材料,因其具有体积小、比重轻、溶解性好、结构多样化以及易于裁剪、调控和加工成型等优点成为化学研究中热门的研究领域之一。回顾其研究历程,早期研究主要聚焦于合成具有高磁相变温度(TC)的分子基磁体。近年来,具有磁化强度慢磁弛豫作用(magnetization relaxation)的分子纳米磁体,即单分子磁体(SMMs)和单链磁体(SCMs),因在高密度信息存储、量子计算等领域具有巨大的潜在应用价值,成为分子磁性材料领域新的研究热点。
氮氧自由基因其较好的稳定性常被用于设计合成分子磁性材料,常用的有Ullman型自由基(Nitronyl-nitroxide,简称NIT或NN)及N-叔丁基氮氧自由基(N-tert-butylnitroxide)。1989年,意大利的D.Gatteschi课题组以Ullman型氮氧自由基作为配体合成分子基磁体,得到了首例氮氧自由基桥联金属形成的分子基铁磁体Mn(hfac)2NIT-i-Pr,使得氮氧自由基-金属配合物逐渐成为分子磁学领域的研究热点。2001年,D.Gatteschi等人成功地将氮氧自由基引入分子纳米磁体的合成,报道了首例在低温下具有超顺磁特性的一维链状配合物[Co(hfac)2(NITPhOMe)]n,由此,氮氧自由基-金属配合物在构筑分子纳米磁体领域受到越来越多的关注。
在各种改善分子纳米磁体性能的化学途径中,自由基因其组成,结构及组装方式等的多样性特点,特别是自由基本身作为自旋载体,可以直接和金属离子配位,进而产生尽可能强的磁交换耦合作用使得自由基-金属配合物成为制备分子纳米磁体的一个重要途径。
发明内容
本发明要解决的技术问题在于克服现有技术的不足,提供一种制备新型稀土-镍混金属分子基磁性材料的方法。
本发明采用氮氧自由基为配体与稀土及过渡金属反应来设计合成自由基-稀土-过渡金属配合物。一方面稀土离子的存在会使体系具有强的磁各向异性;另一方面,氮氧自由基与稀土和过渡金属直接配位可能会产生较强的磁交换耦合,得到结构和性质新颖的分子纳米磁体。
该方法包含以下步骤:
(1)将稀土的六氟乙酰丙酮稀土盐Ln(hfac)X(Ln指稀土离子,X为整数)和Ni(hfac)2(或其水合物)加入正己烷中加热回流,溶液降温至65℃。
(2)在此温度下缓慢加入溶有NIT-4py自由基配体的含有有机溶剂的溶液,加热搅拌反应15min后冷却至室温,待溶剂挥发后,得到方块状晶体。
优选的步骤(1)中稀土的六氟乙酰丙酮稀土盐Ln(hfac)X(Ln指稀土离子,X为整数)和Ni(hfac)2(或其水合物)摩尔比为1:1;优选的步骤(1)中所述稀土的六氟乙酰丙酮盐Ln(hfac)3为镧系金属中的一种,进一步所述镧系金属优选为钆Gd、铽Tb、镝Dy;优选步骤(1)中溶液降温至45-70℃;优选的步骤(2)中NIT-4py自由基配体与稀土的六氟乙酰丙酮盐Ln(hfac)3的摩尔比为1:1;优选的步骤(2)中的有机溶剂是二氯甲烷、三氯甲烷、石油醚、乙醚等常规有机溶剂。
本发明提供的制备稀土-镍分子基磁性材料制备方法简单,可实现大规模的生产,具有广阔的商业化前景。
本发明的另一目的在于提供了利用该方法制备的稀土-镍分子基磁性材料。
本发明制备出的稀土-镍分子基磁性材料能够用于高密度信息存储、量子计算等领域。
具体实施方式
下面通过实施例对本发明进行具体描述,有必要在此指出的是本实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,该领域的技术熟练人员可以根据以上发明的内容做出一些非本质的改进和调整。在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。
实施例1,[Gd(hfac)3Ni(hfac)2NIT-4py(H2O)2](配合物1)的制备:
(1)将Gd(hfac)3·2H2O(0.016g,0.02mmol)和Ni(hfac)2·2H2O(0.0084g,0.02mmol)加入20ml正己烷中加热回流2小时,溶液降温至65℃。
(2)在此温度下缓慢加入溶有NIT-4py自由基配体(0.005g,0.02mmol)的二氯甲烷溶液,加热搅拌反应15min后冷却至室温,静置几天后得到蓝紫色方块状晶体。
产率:43%.Anal.Calc.for C37H25F30GdN3NiO14:C 3.21,H 1.66,N 2.76;Found:C30.06,H 2.45,N 2.89;FT-IR(KBr,cm-1):3392(m),1647(s),1504(m),1375(m),110(s),1198(s),1137(s),801(m),661(m),587(m)cm-1。
实施例2,[Tb(hfac)3Ni(hfac)2NIT-4py(H2O)2](配合物2)的制备:
(1)将Tb(hfac)3·2H2O(0.02mmol)和Ni(hfac)2·2H2O(0.0084g,0.02mmol)加入20ml正己烷中加热回流2小时,溶液降温至65℃。
(2)在此温度下缓慢加入溶有NIT-4py自由基配体(0.005g,0.02mmol)的二氯甲烷溶液,加热搅拌反应15min后冷却至室温,静置几天后得到蓝紫色方块状晶体。
产率:42%.Anal.Calc.for C37H25F30TbN3NiO14:C 3.18,H 1.65,N 2.76;Found:C3.36,H 1.88,N 2.89;FT-IR(KBr,cm-1):3393(m),1648(s),1503(m),1375(m),111(s),1201(s),1138(s),802(m),661(m),586(m)cm-1。
实施例3,[Dy(hfac)3Ni(hfac)2NIT-4py(H2O)2](配合物3)的制备
(1)将Dy(hfac)3·2H2O(0.02mmol)和Ni(hfac)2·2H2O(0.0084g,0.02mmol)加入20ml正己烷中加热回流2小时,溶液降温至65℃。
(2)在此温度下缓慢加入溶有NIT-4py自由基配体(0.005g,0.02mmol)的二氯甲烷溶液,加热搅拌反应15min后冷却至室温,静置几天后得到蓝紫色方块状晶体。
产率:45%.Anal.Calc.for C37H25F30DyN3NiO14:C 3.11,H 1.65,N 2.75;Found:C3.46,H 1.56,N 3.05;FT-IR(KBr,cm-1):3396(m),1649(s),1502(m),1375(m),110(s),1200(s),1137(s),801(m),661(m),588(m)cm-1。
以上所述仅是本发明的较佳实施例,并非对本发明任何形式上的限制,任何熟悉本专利的技术人员在不脱离本发明技术方案范围内,当可利用上述提示的技术内容作出些许更动或修饰为等同条件的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化与修饰,均仍属于本发明方案的范围内。
晶体结构的测定
配合物的结构数据使用Rigaku Saturn型CCD X-射线单晶衍射仪进行了收集,采用扫描方式收集衍射点。基于F2全矩阵最小二乘法修正晶体的坐标以及它们的各向异性热参数,直接法解出非氢原子并通过理论加氢得到氢原子的位置。所有的计算和修正均使用SHELXS-97及SHELXL-97程序进行。配合物的晶体学参数列于表1,主要键长键角数据列于表2。
Table 1Crystal data and structure refinement for complexes 1-3.
2.2配合物[[Ln(hfac)3Ni(hfac)2NIT-4py(H2O)2][LnIII=Gd(1),Tb(2),Dy(3)]的晶体结构描述Table 3SHAPE analysis for complexes1-3.
如图1所示,X-射线单晶解析表明配合物1-3同构,属于三斜晶系,Pī空间群。以配合物1为例描述它们的晶体结构,如图1所示,NIT-4py自由基通过NO基团的O原子和吡啶N原子分别与Gd(III)离子和Ni(II)离子配位形成双核结构。其中,Gd(III)为O8配位模式,六个O原子来自三个hfac配体,一个O原子来自NO基团,还有一个O原子来自配位水分子。Gd-O(hfac)键长在范围内,Gd-O(H2O)键长为Gd-O(rad)键长为与文献报道的Ln-O(Rad)键长一致[6-8]。Ni(II)离子为O5N配位模式,配位原子分别为来自于两个hfac的四个O原子,配位水分子提供的一个O原子,以及一个吡啶N原子。Ni-O(H2O)键长为Ni-N键长为Ni-O(hfac)键长在范围内。Gd-O-N键角为137.9(5)°。用SHAPE软件[15,16]分析了配合物中金属离子的配位构型(Table 3),结果表明Gd(III)配位构型为D4d对称性。分子内Gd…Ni距离为配合物1的晶体空间堆积如图2所示,分子间最短Gd…Gd距离为最短Gd…Ni距离为最短Ni…Ni距离为分子间未配位的NO基团之间的最短距离为如此近的NO…NO距离可能会导致显著的分子间磁相互作用的产生。除了NO基团之间的距离,自由基的π*轨道取向也是影响未配位NO基团之间磁相互作用的重要因素,与此相关的结构参数是两个分子中的N-O···N夹角(α)以及相邻两个分子中未配位的两个NO基团构成的平面与其中一个分子的(ON-C-NO)平面之间的二面角(β)。对于配合物1,其α角为111.62°,β角为83.00°(如图3所示)。
Claims (9)
1.一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:
包含以下步骤,
(1)将六氟乙酰丙酮稀土盐Ln(hfac)X(Ln指稀土离子,X为整数)和Ni(hfac)2或其水合物加入正己烷中加热回流,溶液降温至65℃;
(2)在此温度下缓慢加入溶有NIT-4py自由基配体的含有有机溶剂的溶液,加热搅拌反应15min后冷却至室温,静置待溶液缓慢挥发,得到目标产物的晶体形态。
2.根据权利要求1所述的一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:所述稀土的六氟乙酰丙酮稀土盐Ln(hfac)X和Ni(hfac)2或其水合物摩尔比为1:1。
3.根据权利要求1所述的一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:所述稀土的六氟乙酰丙酮稀土盐Ln(hfac)3为镧系金属中的一种或几种。
4.根据权利要求3所述的一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:所述镧系金属为钆Gd、铽Tb、镝Dy。
5.根据权利要求1所述的一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:步骤(1)中溶液降温至45-70℃。
6.根据权利要求1所述的一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:步骤(2)中NIT-4py自由基配体与稀土的六氟乙酰丙酮盐Ln(hfac)3的摩尔比为1:1。
7.根据权利要求1所述的一种稀土-镍混金属分子基磁性材料的合成方法,其特征在于:步骤(2)中的有机溶剂是指二氯甲烷、三氯甲烷、甲苯、石油醚、乙醚等常规有机溶剂。
8.根据权利要求1所述的方法制备出的稀土-镍混金属分子基磁性材料。
9.根据权利要求1所述的方法制备出的稀土-镍混金属分子基磁性材料用于高密度信息存储或量子计算等。
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