钴酸锶薄膜的结构调控及其性质研究

钙钛矿(Perovskite, P)结构过渡金属氧化物由于其电荷、自旋、轨道、晶体结构等自由度之间的复杂相互作用，展现出多样的性质，例如锰氧化物的磁阻效应、铁氧化物的多铁性、镍氧化物的超导性，从而在存储、铁电、铁磁、超导等领域具有重要应用。它们的基本结构是由氧八面体堆积而成，通式为ABO_3-δ (A位为Ln、Ca、Sr、Ba、Bi 等元素，B位为Ti、Mn、Fe、Co、Ni等过渡金属元素，3-δ为氧含量，δ为氧空位含量)。

SrCoO_3-δ (SCO)因其可变的氧含量，伴随着可控的电学、磁学、光学、电催化等性质，而受到广泛关注。通过高温气氛退火、化学处理、离子液体调控、应力调控等手段，可以控制SCO氧含量在2.5 ~ 3的范围内变化，其晶体结构在钙钛矿(2.75 < 3-δ < 3)和钙铁石(Brownmillerite, BM, 2.5 ≤ 3-δ < 2.75)之间转变。然而，Co⁴⁺离子的不稳定性使得制备和保持氧含量为3的P-SCO极为困难。另一方面，尽管此前有基于BM-SCO，经氢化、脱水处理制备SrCoO₂的报道，但目前的调控手段难以控制SCO的氧含量在2 ~ 2.5范围内连续变化，因此对氧含量在该范围内的SCO的研究仍有待开展。此外，这些调控都基于拓扑化学相变，反应前后SCO在成分、结构、性质上具有较大的连续性，而突破SCO母相结构对称性的相变调控研究较为匮乏。

本论文以钙钛矿结构的SCO薄膜为研究对象，采取空穴/电子掺杂的策略，对SCO的成分、晶体结构及其物理、化学性质进行调控。一方面，从O离子、B位离子和A位离子三方面入手进行非中性调控，分别为：电压驱动调节氧含量、低价Cu取代高价Co进行空穴掺杂、高价Nd取代低价Sr进行电子掺杂。在此基础上，采用应力调控进一步调控Cu或Nd离子掺杂SCO的氧含量和晶体结构。另一方面，采用中性掺杂策略，即在BM-SCO中引入H₂O分子，突破BM-SCO结构对称性的限制，获得具有高电导和优异热电性能的新型层状氧化物。主要内容如下：

首先采用电压调控的手段，快速、连续、可逆地调节SCO的氧含量在2.5 ~ 3的范围内变化，实现SCO在BM-P之间可控相变，并伴随绝缘体-金属、反铁磁-铁磁、透明-不透明等性质的转变。

接着，在B位以低价Cu取代高价Co进行空穴掺杂，Cu的引入，显著降低了SCO薄膜的氧含量，当掺杂浓度超过33%时，氧含量降至2.25以下，形成有三维氧空位通道的新结构；该薄膜展现出增强的导电性和优异的电解水催化性能。另一方面，在A位以高价Nd取代低价Sr进行电子掺杂，Nd的引入，提高了SCO的氧含量并稳定了P相结构，然而其电导率和磁性有所降低。

在此基础上，对Cu或Nd掺杂的SCO薄膜进行应力调控。对Cu掺杂SCO薄膜，由无应力状态逐渐增大压应力或张应力，薄膜中氧含量升高，从具有三维氧空位通道的结构转变为BM相；特别的是，压应力可以减小薄膜的带隙，使其电导率进一步提升。对Nd掺杂的SCO薄膜，当其面内晶格被压缩时，磁性获得增强，电导率提高并且由绝缘态转变为金属态。

我们通过非中性掺杂的策略，实现了对SCO薄膜氧含量、晶体结构和性质的有效调控。但是，这些新的晶体结构依然没有逃脱钙钛矿结构的藩篱。因此在论文的最后，我们采用中性掺杂的策略，即在BM-SCO中引入H₂O，实现了由BM-SCO到新型层状氧化物SrCoO₃H的相变，该材料展现出优异的导电性和热电性能。这一策略有效突破了钙钛矿结构拓扑化学相变的限制，发现了新的钙钛矿氧化物的改性策略。

Perovskite transition metal oxides exhibit diverse properties due to the complex interactions among the degrees of freedom of charge, spin, orbitals, and crystal structures, such as magnetoresistance effect in manganese oxides, multiferroicity in iron oxides, and newly discovered superconductivity in nickel oxides, resulting in important applications in the fields of storage, ferroelectricity, ferromagnetism, superconductivity, and so on. Their basic structure consists of oxygen octahedral stacking with the general formula ABO_3-δ (A-site for elements such as Ln, Ca, Sr, Ba, Bi, etc., B-site for transition metal elements such as Ti, Mn, Fe, Co, Ni, etc., 3-δ is the oxygen content and δ is the oxygen vacancy concentration).

SrCoO_3-δ has attracted attention due to its variable oxygen content accompanied by controllable electrical, magnetic, optical, and electrocatalytic properties. By means of high-temperature atmosphere annealing, chemical treatment, ionic liquid modulation, and stress modulation, the oxygen content of SCO can be tuned in the range of 2.5 ~ 3, and its crystal structure is transformed between P (2.75 < 3-δ < 3) and BM (2.5 ≤ 3-δ < 2.75). However, it is difficult to prepare and stabilize P-SCO with an oxygen content of 3 due to the instability of Co⁴⁺. On the other hand, although the preparation of SrCoO₂ by hydrogenation followed by dehydration of BM-SCO has been reported, it is difficult to control the oxygen content of SCO to vary in the range of 2 ~ 2.5. The SCO with oxygen content in the range of 2 ~ 2.5 still remains to be investigated. In addition, these modulations are based on topological chemical phase transformation, and there is a large continuity in the composition, structure and properties of SCO before and after the reaction. There is a lack of phase-transition modulation studies that break through the structural symmetry of the SCO parent phase.

In this thesis, the perovskite SCO thin films are investigated by adopting the strategy of hole/electron doping to modulate their composition, crystal structure, as well as physical and chemical properties. On the one hand, non-neutral modulation was carried out from O ions, B-site ions and A-site ions, which are: voltage-driven modulation of oxygen content, hole doping by replacing high-valent Co with low-valent Cu, and electron doping by replacing low-valent Sr with high-valent Nd. On this basis, strain engineering was employed to further tune the oxygen content and crystal structure of Cu-doped and Nd-doped SCO. On the other hand, a neutral doping strategy, i.e., the introduction of H₂O into BM-SCO, was employed to break through the structural symmetry of BM-SCO and obtain novel layered oxides with high conductivity and excellent thermoelectric properties. The main contents are as follows:

Firstly, a voltage-driven way was employed to quickly, continuously and reversibly tune the oxygen content of SCO to vary in the range of 2.5 ~ 3, realizing the controlled phase transformation of SCO between BM-P, accompanied with the property transition of insulator-metal, antiferromagnetic-ferromagnetic and transparency-opacity.

Next, high-valent Co was replaced by low-valent Cu for hole doping at the B-site. The introduction of Cu significantly reduced the oxygen content of the SCO film to below 2.25 when the concentration of Cu exceeded 33%, forming a new structure with three-dimensional oxygen vacancy channels; the film exhibited enhanced electrical conductivity and excellent catalytic performance for electrolytic water. On the other hand, electron doping was carried out by replacing low-valent Sr with high-valent Nd at the A-site. The introduction of Nd increased the oxygen content of SCO and stabilized the P structure; however, its conductivity and magnetic properties were reduced.

On this basis, strain engineering was used on Cu-doped and Nd-doped SCO films. For Cu-doped SCO, when compressive or tensile strain increased, the oxygen content in the films was elevated and transformed SCO from a structure with three-dimensional oxygen vacancy channels to the BM; in particular, the compressive strain reduced the bandgap of the films, which led to a further enhancement of their conductivity. For Nd-doped SCO, when the in-plane lattice was compressed, the magnetic properties were enhanced and the conductivity was increased, resulting in an insulator-metal transition.

We have achieved an effective modulation of the oxygen content, crystal structure and properties of SCO thin films through the non-neutral doping strategy. However, these new crystal structures still have not escaped the fence of perovskite structure. Therefore, at the end of the paper, we adopt a neutral doping strategy, i.e., introducing H₂O into BM-SCO, to realize the phase transition from BM-SCO to a novel layered oxide SrCoO₃H, which exhibited excellent electronic conductivity and thermoelectric properties. This strategy effectively breaks through the limitation of the topological chemical phase transition of perovskite and discovers a new modification strategy for perovskite oxides.

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