典型含氧八面体金属氧化物的高压结构相变研究
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摘要
以稀土倍半氧化物﹑钙钛矿和尖晶石结构氧化物为代表的典型含氧八面体金属氧化物，因其独特的﹑优异的光学、电学﹑热学﹑磁学等性能以及在光学领域、电子器件、多功能材料等方面广泛的应用价值而成为材料科学的研究热点。利用高压极端条件来研究材料的结构和物理性质的变化，是当前高压物理学领域重要的研究方向，对获得新结构﹑合成新材料﹑发现新现象、总结新规律具有重要的指导意义和潜在的应用价值。然而，对于以上三种典型含氧八面体金属氧化物以及氧相关体系的高压结构相变研究目前仍然存在亟待解决的问题，即高压下含氧八面体金属氧化物的新型压致相变和高压新结构的发现以及纳米效应对其相变行为的影响。针对以上问题，我们开展了相关研究工作。
本论文以稀土倍半氧化物、钙钛矿氧化物以及尖晶石结构氧化物等几种典型含氧八面体金属氧化物以及限域于单晶分子筛一维纳米孔道内双原子分子氧为主要对象，利用金刚石对顶砧装置对它们开展了详细的高压结构相变研究，获得如下结果：
1）纳米尺寸效应对准一维稀土倍半氧化物以及纳米尖晶石氧化物相变行为的影响和新型压致相变以及异常压缩行为的发现
以稀土倍半氧化物准一维Gd2O3/Er3+纳米棒和尖晶石氧化物Co3O4为例，利用原位高压同步辐射X射线衍射和高压拉曼等实验研究了它们的高压相变行为。发现Gd2O3/Er3+纳米棒经历了不同于体材料和纳米颗粒的相变过程，其并没有发生由立方结构向高压六方相的结构转变，而是转变为一种非晶结构。利用TEM观测了样品加压前和卸压后的形貌变化，发现卸压后的样品仍然能够保持原始样品的棒状形貌。这是首次在Gd2O3/Er3+一维纳米材料中发现了压致非晶化现象。这一实验结果进一步深化了纳米尺寸效应以及特殊形貌对稀土倍半氧化物纳米晶高压结构相变行为的认识。对比研究了典型尖晶石氧化物Co3O4体/纳米材料的高压相变行为，发现了Co3O4体材料和纳米材料高压下完整的相转变行为。并且，观测到了Co3O4纳米材料的体积不连续变化这一异常的压缩行为。经研究分析，Co3O4尖晶石结构中独特的阳离子排布以及纳米材料的高表面能等纳米效应是影响Co3O4高压行为的主要因素。这些实验结果丰富了对纳米尖晶石高压行为的认识，同时对材料相变机制以及制备新功能材料具有重要的指导意义。
2）发现了钙钛矿氧化物的新型重构式结构相变和高压新相
以钙钛矿氧化物CaZrO3和BaZrO3为例，利用原位高压同步辐射X光衍射方法研究了它们的高压相变行为。在高达50GPa的压力范围内，发现了正交相CaZrO3可以稳定保持至30GPa，之后其发生了由正交结构向高压新相-单斜相的结构相变。这是首次发现CaZrO3的高压新相，其相变行为不同于先前研究报道的其他钙钛矿氧化物的相变行为，是一种新型的重构式结构相变。ZrO6八面体的旋转或倾斜在CaZrO3的高压行为中发挥重要的作用。发现立方相BaZrO3在压力达到17.2GPa时，发生了从立方相（空间群为Pm3m）到四方相（空间群为I4/mcm）的转变。这是首次在实验中观测到BaZrO3的结构相变。这些实验结果使我们对钙钛矿氧化物的结构转变行为有了新的认识，极大地丰富了钙钛矿氧化物相转变的内容。
3）发现了压力作用下限域于AlPO4-5一维纳米孔道内氧的新型结构转变
利用原位高压同步辐射和高压拉曼光谱技术，以单晶分子筛AFI为模板，以限域于单晶分子筛孔道内双原子分子氧为例，首次开展了限域于纳米孔道内氧的高压行为研究。对比研究了限域于AFI纳米孔道内部氧和体材料氧的高压行为。观察到在6.0GPa左右，氧的拉曼振动模式发生了明显了的变化，对比体材料氧在此压力区间发生的由液态-β相（6.0GPa）的相变，发现限域于分子筛内部的氧经历了液态氧-γ相氧的转变，表明限域氧的高压行为明显不同于体材料氧。这是利用限域的方法，首次在常温条件下获得了低温条件下存在的γ-O2。XRD实验结果表明AFI的非晶化转变压力由8.5GPa明显提高到17.5GPa，进一步表明利用高压手段将氧成功限域到AFI纳米孔道中。此实验结果对高压下纳米限域体系等纳米功能材料的设计具有重要的指导意义，并对小分子的捕获和储存方面有重要的应用前景。
Due to the unique and excellent chemical and physical properties and extensivepotential applications in the fields of optical, electronic device and multi-functionalmaterials, metal oxides, such as rare earth sesquioxide, perovskite oxides and spineloxides have been the subject of intense studies. The studies on the structural phasetransition and physical properties of materials by means of high pressure experimentaltechnology have been an important research subject in high pressure physical science,and it has important scientific significance and potential application value forobtaining new structures, synthesizing new materials, discovering new phenomenaand revealing new rules. However, there still exists some urgent problems to solve inthe pressure-induced phase transition studies of the above mentioned three typicalmetal oxides containing oxygen octahedral and oxygen, including the new type ofpressure-induced phase transitions, novel high pressure structures of metal oxidescontaining oxygen octahedra and the influence of nano effects on the phase transitionbehavior. Therefore, we carried out the related researches about the above mentionedproblems.
In this thesis, we performed high pressure experimental researches on severaltypical metal oxide materials, such as rare earth sesquioxide, perovskite oxides andspinel oxides by using diamond anvil cell (DAC) to make detailed studies on theirstructural phase transitions under pressure. In addition, we study the high pressurebehavior of oxygen confined in the one-dimensional nano channels of AFI by in situhigh pressure experiments.
1) The influence of nano effects on the phase transitions of one-dimensionalrare-earth sesquioxides nanomaterials and spinel oxides nanomaterials, and discoveries of new type of pressure-induced transition and abnormal compressionbehavior.
Taking the rare-earth sesquioxides Gd2O3/Er3+nanorods and spinel oxides Co3O4as typical examples, we have performed high pressure studies by using in situsynchrotron X-ray diffraction and Raman spectroscopy. Compared with the bulkmaterials and nanoparticles, we found that Gd2O3/Er3+nanorods undergo a differentphase transition process. The experimental results show that it does not transformform cubic phase to hexagonal phase under high pressure, but transforms into anamorphous phase. The TEM observation of the quenched samples clearly shows thatthe samples almost maintain their pristine nanorod shape. This is the first time that wediscovered the pressure-induced amorphous structure in the Gd2O3/Er3+nanorods. Theexperimental results provide a further understanding of the influence of nano effectsand special morphology on the phase transition behavior of rare-earth sesquioxides.For spinel oxides Co3O4, we found the complete phase transition process. Importantly,it is found the abnormal compression behavior of the discontinuous volume change inCo3O4nanomaterials. It is suggested that the unique cation distribution and thenano-size effect play vital roles in the high pressure behaviors of Co3O4. These resultsenrich the understanding of high pressure behavior in nano spinels and have animportant significance of the phase transition mechanism and preparation of newfunctional materials.
2) Discoveries of a new type of reconstructive phase transition and new highpressure phases in perovskites.
Taking CaZrO3and BaZrO3perovskites as examples, we have performed thehigh pressure studies by using in situ synchrotron X-ray diffraction. In the study of thehigh pressure behavior of CaZrO3up to50.1GPa, we found that the orthorhombicphase CaZrO3can be stable up to30GPa, then it transforms into a new high pressuremonoclinic structure. This new high pressure phase of CaZrO3is found for the firsttime, and it is different from the high pressure structures that were reported for theother perovskite oxides in previous studies. It is a new type of reconstructive phase transition. In addition, we found that a phase transition from cubic phase (Pm3m) totetragonal phase (I4/mcm) takes place at a pressure of17.2GPa in BaZrO3. This phasetransition was found for the first time. It is proposed that the distorted and rotation ortilting of octahedra play an important role in the high pressure behavior of perovskites.These results provide a new understanding of phase transition behaviors of perovskiteoxides and greatly enrich the content of phase transition of perovskite oxides.
3）Discovery of the new structure change of oxygen confined in the channels ofAlPO4-5under high pressure.
The high pressure behaviors of oxygen confined inside the AFI channels havebeen studies by in situ X-ray diffraction and Raman spectroscopy for the first time. Itis found that the liquid oxygen solidifies to β phase in bulk oxygen at about6.0GPa.Compared with bulk oxygen, the Raman mode of confined oxygen has an obviouschange at6.0GPa. The result indicates that the confined oxygen undergoes a phasetransition from liquid oxygen to γ phase at6.0GPa. We obtained the low temperatureγ-O2through the confinment effect for the first time. In addition, the XRD experimentresults show that the transition pressure of crystalline-to-amorphous phase transitionfor AFI obviously increased from8.5GPa to17.5GPa, indicating that oxygenmolecules can be inserted into the channels of AFI single crystals. The experimentalresults show a great significance for designing the one-dimensional nanometerfunctional materials and an important application prospect for the capture and storageof small molecules.
本论文以稀土倍半氧化物、钙钛矿氧化物以及尖晶石结构氧化物等几种典型含氧八面体金属氧化物以及限域于单晶分子筛一维纳米孔道内双原子分子氧为主要对象，利用金刚石对顶砧装置对它们开展了详细的高压结构相变研究，获得如下结果：
1）纳米尺寸效应对准一维稀土倍半氧化物以及纳米尖晶石氧化物相变行为的影响和新型压致相变以及异常压缩行为的发现
以稀土倍半氧化物准一维Gd2O3/Er3+纳米棒和尖晶石氧化物Co3O4为例，利用原位高压同步辐射X射线衍射和高压拉曼等实验研究了它们的高压相变行为。发现Gd2O3/Er3+纳米棒经历了不同于体材料和纳米颗粒的相变过程，其并没有发生由立方结构向高压六方相的结构转变，而是转变为一种非晶结构。利用TEM观测了样品加压前和卸压后的形貌变化，发现卸压后的样品仍然能够保持原始样品的棒状形貌。这是首次在Gd2O3/Er3+一维纳米材料中发现了压致非晶化现象。这一实验结果进一步深化了纳米尺寸效应以及特殊形貌对稀土倍半氧化物纳米晶高压结构相变行为的认识。对比研究了典型尖晶石氧化物Co3O4体/纳米材料的高压相变行为，发现了Co3O4体材料和纳米材料高压下完整的相转变行为。并且，观测到了Co3O4纳米材料的体积不连续变化这一异常的压缩行为。经研究分析，Co3O4尖晶石结构中独特的阳离子排布以及纳米材料的高表面能等纳米效应是影响Co3O4高压行为的主要因素。这些实验结果丰富了对纳米尖晶石高压行为的认识，同时对材料相变机制以及制备新功能材料具有重要的指导意义。
2）发现了钙钛矿氧化物的新型重构式结构相变和高压新相
以钙钛矿氧化物CaZrO3和BaZrO3为例，利用原位高压同步辐射X光衍射方法研究了它们的高压相变行为。在高达50GPa的压力范围内，发现了正交相CaZrO3可以稳定保持至30GPa，之后其发生了由正交结构向高压新相-单斜相的结构相变。这是首次发现CaZrO3的高压新相，其相变行为不同于先前研究报道的其他钙钛矿氧化物的相变行为，是一种新型的重构式结构相变。ZrO6八面体的旋转或倾斜在CaZrO3的高压行为中发挥重要的作用。发现立方相BaZrO3在压力达到17.2GPa时，发生了从立方相（空间群为Pm3m）到四方相（空间群为I4/mcm）的转变。这是首次在实验中观测到BaZrO3的结构相变。这些实验结果使我们对钙钛矿氧化物的结构转变行为有了新的认识，极大地丰富了钙钛矿氧化物相转变的内容。
3）发现了压力作用下限域于AlPO4-5一维纳米孔道内氧的新型结构转变
利用原位高压同步辐射和高压拉曼光谱技术，以单晶分子筛AFI为模板，以限域于单晶分子筛孔道内双原子分子氧为例，首次开展了限域于纳米孔道内氧的高压行为研究。对比研究了限域于AFI纳米孔道内部氧和体材料氧的高压行为。观察到在6.0GPa左右，氧的拉曼振动模式发生了明显了的变化，对比体材料氧在此压力区间发生的由液态-β相（6.0GPa）的相变，发现限域于分子筛内部的氧经历了液态氧-γ相氧的转变，表明限域氧的高压行为明显不同于体材料氧。这是利用限域的方法，首次在常温条件下获得了低温条件下存在的γ-O2。XRD实验结果表明AFI的非晶化转变压力由8.5GPa明显提高到17.5GPa，进一步表明利用高压手段将氧成功限域到AFI纳米孔道中。此实验结果对高压下纳米限域体系等纳米功能材料的设计具有重要的指导意义，并对小分子的捕获和储存方面有重要的应用前景。
Due to the unique and excellent chemical and physical properties and extensivepotential applications in the fields of optical, electronic device and multi-functionalmaterials, metal oxides, such as rare earth sesquioxide, perovskite oxides and spineloxides have been the subject of intense studies. The studies on the structural phasetransition and physical properties of materials by means of high pressure experimentaltechnology have been an important research subject in high pressure physical science,and it has important scientific significance and potential application value forobtaining new structures, synthesizing new materials, discovering new phenomenaand revealing new rules. However, there still exists some urgent problems to solve inthe pressure-induced phase transition studies of the above mentioned three typicalmetal oxides containing oxygen octahedral and oxygen, including the new type ofpressure-induced phase transitions, novel high pressure structures of metal oxidescontaining oxygen octahedra and the influence of nano effects on the phase transitionbehavior. Therefore, we carried out the related researches about the above mentionedproblems.
In this thesis, we performed high pressure experimental researches on severaltypical metal oxide materials, such as rare earth sesquioxide, perovskite oxides andspinel oxides by using diamond anvil cell (DAC) to make detailed studies on theirstructural phase transitions under pressure. In addition, we study the high pressurebehavior of oxygen confined in the one-dimensional nano channels of AFI by in situhigh pressure experiments.
1) The influence of nano effects on the phase transitions of one-dimensionalrare-earth sesquioxides nanomaterials and spinel oxides nanomaterials, and discoveries of new type of pressure-induced transition and abnormal compressionbehavior.
Taking the rare-earth sesquioxides Gd2O3/Er3+nanorods and spinel oxides Co3O4as typical examples, we have performed high pressure studies by using in situsynchrotron X-ray diffraction and Raman spectroscopy. Compared with the bulkmaterials and nanoparticles, we found that Gd2O3/Er3+nanorods undergo a differentphase transition process. The experimental results show that it does not transformform cubic phase to hexagonal phase under high pressure, but transforms into anamorphous phase. The TEM observation of the quenched samples clearly shows thatthe samples almost maintain their pristine nanorod shape. This is the first time that wediscovered the pressure-induced amorphous structure in the Gd2O3/Er3+nanorods. Theexperimental results provide a further understanding of the influence of nano effectsand special morphology on the phase transition behavior of rare-earth sesquioxides.For spinel oxides Co3O4, we found the complete phase transition process. Importantly,it is found the abnormal compression behavior of the discontinuous volume change inCo3O4nanomaterials. It is suggested that the unique cation distribution and thenano-size effect play vital roles in the high pressure behaviors of Co3O4. These resultsenrich the understanding of high pressure behavior in nano spinels and have animportant significance of the phase transition mechanism and preparation of newfunctional materials.
2) Discoveries of a new type of reconstructive phase transition and new highpressure phases in perovskites.
Taking CaZrO3and BaZrO3perovskites as examples, we have performed thehigh pressure studies by using in situ synchrotron X-ray diffraction. In the study of thehigh pressure behavior of CaZrO3up to50.1GPa, we found that the orthorhombicphase CaZrO3can be stable up to30GPa, then it transforms into a new high pressuremonoclinic structure. This new high pressure phase of CaZrO3is found for the firsttime, and it is different from the high pressure structures that were reported for theother perovskite oxides in previous studies. It is a new type of reconstructive phase transition. In addition, we found that a phase transition from cubic phase (Pm3m) totetragonal phase (I4/mcm) takes place at a pressure of17.2GPa in BaZrO3. This phasetransition was found for the first time. It is proposed that the distorted and rotation ortilting of octahedra play an important role in the high pressure behavior of perovskites.These results provide a new understanding of phase transition behaviors of perovskiteoxides and greatly enrich the content of phase transition of perovskite oxides.
3）Discovery of the new structure change of oxygen confined in the channels ofAlPO4-5under high pressure.
The high pressure behaviors of oxygen confined inside the AFI channels havebeen studies by in situ X-ray diffraction and Raman spectroscopy for the first time. Itis found that the liquid oxygen solidifies to β phase in bulk oxygen at about6.0GPa.Compared with bulk oxygen, the Raman mode of confined oxygen has an obviouschange at6.0GPa. The result indicates that the confined oxygen undergoes a phasetransition from liquid oxygen to γ phase at6.0GPa. We obtained the low temperatureγ-O2through the confinment effect for the first time. In addition, the XRD experimentresults show that the transition pressure of crystalline-to-amorphous phase transitionfor AFI obviously increased from8.5GPa to17.5GPa, indicating that oxygenmolecules can be inserted into the channels of AFI single crystals. The experimentalresults show a great significance for designing the one-dimensional nanometerfunctional materials and an important application prospect for the capture and storageof small molecules.
引文
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