高压下A~(2+)Nb_2O_6（A~(2+)=Ca、Zn、Mg）的结构转变研究
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摘要
高压研究可以发现物质在常压和室温下不能表现出来的一些现象，进而揭示新规律、新性质，乃至发现新物质。随着静高压原位技术的迅猛发展，金刚石对顶砧（DAC）已被广泛应用于各种物质的高压物性研究。压力诱导相变，化学反应及新结构的形成越来越引起国内外科研人员的关注。作为热力学的一个基本参数，压力与被压缩物质的总能量相关，通过改变压力可以控制相组成及反应路径，这是由于压力能非常有效地缩短物质内部的原子(分子)间距离、增加相邻电子轨道重叠，进而改变电子结构和原子(分子)间的相互作用，使之达到一个新的强制高压平衡态。如果在这个压力下，强制高压平衡态中有原子重排和对称性改变，这个强制高压平衡态就是一个新的高压相，这种晶体结构转变称为压力诱导的相变。拉曼光谱，同步辐射光谱与高压技术相结合使人们可以方便的研究在压力作用下的物质内部结构变化，其中高压原位拉曼光谱是目前最常用的高压实验技术之一，为研究物质在高压下的相变和化学反应提供了一个非常灵敏和有效的探测手段。
近年来,对钶铁矿结构的高压动力学和相转化的研究引起了越来越多的兴趣。目前,高压下钶铁矿结构的相变研究己有一些报导。
具有A~(2+)Nb_2O_6（A=Ca, Mg, Zn, Fe, Ni, Cd, Co，Mn）化学式的二元铌酸盐，都具有钶铁矿结构。A~(2+)Nb_2O_6铌酸盐系列材料，在其结构中同时具有NbO_6和AO_6两种八面体基团，特殊的结构使其具有优良的压电、铁电性能、荧光和微波介电性能，此外还具有非线性光学效应、电光效应及光折射效应。因此在压电和热释电器件、激光倍频、电光调制、光记忆、光计算、荧光和微波介电材料等方面具有潜在的应用前景。
几个钶铁矿结构，如NaNbO_3和(Fe, Mn)(Nb, Ta)_2O_6，在高压下的结构研究有过文献报道。高压下研究物质的结构相变是有重要意义的。本文首次利用金刚石对顶砧技术分别对CaNb_2O_6在20GPa以下压力范围、ZnNb_2O_6和MgNb_2O_6在30GPa以下压力范围的结构变化进行了研究。此外，我们利用Linkam变温实验系统与原位拉曼光谱结合，研究了CaNb_2O_6晶体拉曼光谱对温度的响应程度。
1. CaNb_2O_6晶体高压相变研究：
本文通过原位高压拉曼和同步辐射对CaNb_2O_6晶体粉末在20GPa以下的结构转变进行了研究。拉曼光谱显示多数拉曼峰强度减弱，且随着压力增加向高波数方向移动。压力频移曲线分别在9和15GPa处形成了拐点。ADXRD谱显示在9.4GPa以上有旧峰消失和新峰出现。结果分析表明，CaNb_2O_6钶铁矿结构在压缩过程中发生了一个压致相变，此相变在8GPa左右开始，在15GPa左右完成。结构转变主要表现在沿a轴(CaNbNbCaNbNb层堆积方向)压缩，而沿b轴方向膨胀。为了解析高压新相的详细结构信息，对15.1GPa以上的的原位同步辐射X射线衍射谱进行了精修，得到新相属于单斜结构(P21/c)，晶格参数为a=8.2857A、b=5.92358A、c=4.69152A、β=104.41°。此高压相在23GPa压力以下是稳定的，且压致相变是可逆的。在压力作用下NbO_6和CaO_6八面体变形、NbO_6和CaO_6八面体链的变形是相变的重要原因。
对CaNb_2O_6晶体粉末在-190到530℃范围内进行了变温拉曼研究。结果显示没有新峰的产生，绝大多数的拉曼振动模式呈现阶段的线性变化且变化率不相同，说明不同的化学键振动对温度的响应程度是不相同的。
2. ZnNb_2O_6晶体高压相变研究：
本文通过原位拉曼和原位同步辐射对ZnNb_2O_6晶体在29GPa以下的结构转变进行了研究。拉曼光谱显示在20GPa以下谱线压缩率分段连续，在10GPa和16GPa附近出现拐点，而在20GPa以上基本观察不到明显的拉曼峰。高压原位X射线衍射图谱显示，在压力达到10GPa以上，衍射谱中有峰出现和峰消失现象。分析结果表明，ZnNb_2O_6钶铁矿结构在压缩过程中发生了一个压致相变，此相变在10GPa左右开始，在16GPa左右完成，形成一个高压相；继续增加压力到20GPa以上形成无序态。卸压以后，拉曼光谱恢复至常压状态，表明压致相变和压致无序态都是可逆的。
3. MgNb_2O_6晶体高压相变研究：
本文通过原位拉曼和原位同步辐射对MgNb_2O_6晶体在高压下的结构进行了研究。多数拉曼峰的强度随着压力的增高而呈现出变弱并且移向高波数方向的趋势，在三个阶段均有不同的斜率变化，在8GPa和15GPa附近分别形成拐点。继续加压至22GPa时，拉曼谱发生很大变化，很多峰消失不见。X射线散射图谱显示在9GPa以上时有峰的消失和产生现象。分析结果表明，MgNb_2O_6钶铁矿结构在压缩过程中发生了一个压致相变，此相变在8GPa左右开始，在16GPa左右完成，形成一个高压相；新相是单斜对称，属于空间群P2/C，晶格参数为a=3.56453、 b=14.8218、 c=4.91144，单胞体积是255.1383。继续增加压力到20GPa以上形成无序态。卸压以后，拉曼峰恢复至常压状态，表明了压致相变和压致无序态都是可逆的。
此外，对掺杂1%Eu的MgNb_2O_6晶体在高压下的结构进行了研究。分析结果表明，样品在压缩过程中也发生了一个完整的压致相变，此相变在8GPa左右开始，在15GPa左右完成，相变点略低于未掺杂的MgNb_2O_6晶体。这可以解释为Mg~(2+)的电荷比Eu~(3+)的电荷要低，根据电子补偿原理，格点位置Eu~(3+)代替了Mg~(2+)，导致晶格中有Mg~(2+)四面体空位形成。加压过程中MgO_6八面体也由于Eu~(3+)替代空位的存在而使体积改变更容易发生，因此表现为相变点稍微降低。
上述研究结果对深入了解A~(2+)Nb_2O_6的钶铁矿结构在不同压力下的相变过程及高压下的微结构有重要意义,对常压下拉曼峰的归属和指认都有重要的参考价值，为钶铁矿结构材料在微波介电领域的应用提供了实验依据，也为寻找新功能材料提供了方向。
High-pressure and low-temperature research can discover some newphenomenon which substances cannot exhibit at normal pressure androom temperature, disclose new rules and properties, and even find newsubstances. It provides new approaches for investigating substances’properties at high pressure and low temperature and explaining physicalphenomenon at normal pressure and room temperature. With rapiddeveloping of static high pressure measuring technology, diamond anvilcells (DAC) has been widely applied to the high-pressure study of manymaterials. It is well-known that the application of pressure on crystalsresults in decrease of interatomic distance and increase of the overlappingof the adjacent electron orbit，which will change the electronic structureand the forces of the adjacent atoms. Consequently a forced equilibriumstate under pressure is formed. If there are the rearrangement of atomsand the change of symmetry in it, the forced equilibrium state is a newcrystal structure phase, and the phase transition is named as thepressure-induced phase transition. Raman spectroscopy and x-raydiffraction combined with the high-pressure technology can make us convenient to investigate the structural changes of materials underpressure, so the high-pressure in-situ Raman spectroscopy is one of themost useful high-pressure experimental technologies, and supplies asensitive and effective probing method for investigating phase transitionand chemical reaction of the substance in DAC.
Recently, high pressure study on AB2O_6of columbite structure waswidely applied in the production for industrial chemicals and polymers.Raman spectroscopy and x-ray diffraction combined with thehigh-pressure technology can make us convenient to investigate thestructural changes of materials under pressure. At present, high pressurestudy on niobate had been reported, but so far no has accurate transitionpoint or the structural characterization of their high-pressure phase.
Binary niobate ceramies, with the formula A~(2+)Nb_2O_6where A=Ca, Mg,Zn, Fe, Ni, Cd, Co，Mn, have the orthorhombic columbite structure.There is a growing interest in the columbites as microwave dielectricceramics, due to their lower processing temperatures, less complicatedprocessing, the lower cost of niobium compared with tantalum andlow-temperature cofired ceramics (LTCC) with Cu2+.
Up to now, there are few researches on the crystal structural evolutionof columbites under high pressure. Yosuke Shiratori et al. reported onpressure-induced phase transitions in NaNbO_3by high-pressure Ramanspectroscopy, and found different successive transitions below16GPa. Pistorino et al. and Serena et al. reported on crystal structure of (Fe,Mn)(Nb, Ta)2O_6under high pressure by single-crystal X-ray diffraction,and did not observed phase transition below7GPa. On the crystalstructural evolution of A~(2+)Nb_2O_6under high pressure, there have been noreports. The in-situ high pressure Raman spectroscopy is a very powerfultechnology for dynamically investigating the pressure-induced phasetransition of materials, and the in-situ XRD spectrum is intuitive tocharacterize the crystal structure. In the present work, we have performedin-situ high pressure Raman spectroscopy and in-situ XRD measurementswith a DAC to investigate the pressure-induced phase transition inCaNb_2O_6up to23GPa, ZnNb_2O_6and MgNb_2O_6up to30GPa respectively.Besides, the comparison of crystalline phases obtained by high pressureand by low-temperature crystallization is an important direction of highpressure research. We also studied the Raman peaks of these three niobateat low temperature by in-situ Raman spectroscopy associated withLinkam variable-temperature experimental system, in comparison withtheir pressure-induced phase transition.
The main contents and conclusions as follows:
1. Pressure-induced phase transition in CaNb_2O_6.
We have performed the in-situ high pressure studies of CaNb_2O_6using Raman spectroscopy and Synchrotron X-ray diffraction in aDAC up to23GPa. Both Raman and X-ray diffraction data provide evidence of a reversible phase transition from Pbcn to P21/c,beginning from about8GPa and completing at15GPa. Thecompression is mainly on the a direction of stacking ofCaNbNbCaNbNb layers, and the structure expands along the bdirection. The phase transition involves the deformation andrearrangement of the NbO_6and CaO_6octahedra, as well as thedistortion of the NbO_6and CaO_6octahedral chains. Thehigh-pressure phase keeps stable below22.9GPa. All of thesubsequent XRD patterns above15.1GPa are well described withmonoclinic symmetry, and the indexed lattice parameters area=8.2857, b=5.92358, c=4.69152, β=104.41°by the Pawleyrefinements of the X-ray diffraction data.
Temperature dependence Raman spectra of all the crystals showthat there is no phase transition in the whole temperature range(-190-560℃).The temperature-dependent shift of Raman phononsis also discussed in the context.
2. Pressure-induced phase transition in ZnNb_2O_6.
We have performed the in-situ high pressure studies of ZnNb_2O_6using Raman spectroscopy in a DAC up to30GPa. Raman spectraprovide evidence of a reversible phase transition, beginning fromabout10GPa and completing at16GPa. The high-pressure phase keeps stable below20GPa. With the pressure over20GPa, adisordered state formed.
3. Pressure-induced phase transition in MgNb_2O_6.
In situ x-ray diffraction and Raman spectroscopy were used toexplore the pressure-induced phase transformation of MgNb_2O_6single crystal powder with orthorhombic columbite structure29.4GPa and35.0GPa, respectively. Results indicate that MgNb_2O_6initially transforms to the monoclinic structure at about8GPa, andsuch a phase is completed at about15GPa. Also we identified thephase transition as a space group change from Pbcnto P2/C. Thehigh-pressure phase remained stable up to about22.3GPa. With thepressure over22GPa, a disordered state formed.Besides, we carefully studied the crystal structure of1%molEu3+doped MgNb_2O_6under high pressure. A complete phasetransition initially occurred at about8GPa and ultimatelycompleted at around15GPa was observed, which was slightly lessthan pristine MgNb_2O_6. This is reasonably ascribed to higherelectrons deriving from the substitution of Mg2+by Eu3+. Aftersubstitution, the Mg2+tetrahedron vacancy is formed based uponelectronic compensation principle. Furthermore, the volume ofMgO_6octahedraon was also varied by Eu3+substitution and theexistence of vacancy made the phase transition easily happened. As
mentioned above, a slightly decrease of phase transition wasinvestigated in our study.
In summary, our results not only provide an experimental meansfor deeply understanding the phase transition of A~(2+)Nb_2O_6andmicrostructure under different pressure with columbite structurebut also are great significance for its Raman peaks identificationunder normal pressure. Using these experimental methods, it couldbe greatly helpful for the application of columbite structurematerials and novel functional species.
近年来,对钶铁矿结构的高压动力学和相转化的研究引起了越来越多的兴趣。目前,高压下钶铁矿结构的相变研究己有一些报导。
具有A~(2+)Nb_2O_6（A=Ca, Mg, Zn, Fe, Ni, Cd, Co，Mn）化学式的二元铌酸盐，都具有钶铁矿结构。A~(2+)Nb_2O_6铌酸盐系列材料，在其结构中同时具有NbO_6和AO_6两种八面体基团，特殊的结构使其具有优良的压电、铁电性能、荧光和微波介电性能，此外还具有非线性光学效应、电光效应及光折射效应。因此在压电和热释电器件、激光倍频、电光调制、光记忆、光计算、荧光和微波介电材料等方面具有潜在的应用前景。
几个钶铁矿结构，如NaNbO_3和(Fe, Mn)(Nb, Ta)_2O_6，在高压下的结构研究有过文献报道。高压下研究物质的结构相变是有重要意义的。本文首次利用金刚石对顶砧技术分别对CaNb_2O_6在20GPa以下压力范围、ZnNb_2O_6和MgNb_2O_6在30GPa以下压力范围的结构变化进行了研究。此外，我们利用Linkam变温实验系统与原位拉曼光谱结合，研究了CaNb_2O_6晶体拉曼光谱对温度的响应程度。
1. CaNb_2O_6晶体高压相变研究：
本文通过原位高压拉曼和同步辐射对CaNb_2O_6晶体粉末在20GPa以下的结构转变进行了研究。拉曼光谱显示多数拉曼峰强度减弱，且随着压力增加向高波数方向移动。压力频移曲线分别在9和15GPa处形成了拐点。ADXRD谱显示在9.4GPa以上有旧峰消失和新峰出现。结果分析表明，CaNb_2O_6钶铁矿结构在压缩过程中发生了一个压致相变，此相变在8GPa左右开始，在15GPa左右完成。结构转变主要表现在沿a轴(CaNbNbCaNbNb层堆积方向)压缩，而沿b轴方向膨胀。为了解析高压新相的详细结构信息，对15.1GPa以上的的原位同步辐射X射线衍射谱进行了精修，得到新相属于单斜结构(P21/c)，晶格参数为a=8.2857A、b=5.92358A、c=4.69152A、β=104.41°。此高压相在23GPa压力以下是稳定的，且压致相变是可逆的。在压力作用下NbO_6和CaO_6八面体变形、NbO_6和CaO_6八面体链的变形是相变的重要原因。
对CaNb_2O_6晶体粉末在-190到530℃范围内进行了变温拉曼研究。结果显示没有新峰的产生，绝大多数的拉曼振动模式呈现阶段的线性变化且变化率不相同，说明不同的化学键振动对温度的响应程度是不相同的。
2. ZnNb_2O_6晶体高压相变研究：
本文通过原位拉曼和原位同步辐射对ZnNb_2O_6晶体在29GPa以下的结构转变进行了研究。拉曼光谱显示在20GPa以下谱线压缩率分段连续，在10GPa和16GPa附近出现拐点，而在20GPa以上基本观察不到明显的拉曼峰。高压原位X射线衍射图谱显示，在压力达到10GPa以上，衍射谱中有峰出现和峰消失现象。分析结果表明，ZnNb_2O_6钶铁矿结构在压缩过程中发生了一个压致相变，此相变在10GPa左右开始，在16GPa左右完成，形成一个高压相；继续增加压力到20GPa以上形成无序态。卸压以后，拉曼光谱恢复至常压状态，表明压致相变和压致无序态都是可逆的。
3. MgNb_2O_6晶体高压相变研究：
本文通过原位拉曼和原位同步辐射对MgNb_2O_6晶体在高压下的结构进行了研究。多数拉曼峰的强度随着压力的增高而呈现出变弱并且移向高波数方向的趋势，在三个阶段均有不同的斜率变化，在8GPa和15GPa附近分别形成拐点。继续加压至22GPa时，拉曼谱发生很大变化，很多峰消失不见。X射线散射图谱显示在9GPa以上时有峰的消失和产生现象。分析结果表明，MgNb_2O_6钶铁矿结构在压缩过程中发生了一个压致相变，此相变在8GPa左右开始，在16GPa左右完成，形成一个高压相；新相是单斜对称，属于空间群P2/C，晶格参数为a=3.56453、 b=14.8218、 c=4.91144，单胞体积是255.1383。继续增加压力到20GPa以上形成无序态。卸压以后，拉曼峰恢复至常压状态，表明了压致相变和压致无序态都是可逆的。
此外，对掺杂1%Eu的MgNb_2O_6晶体在高压下的结构进行了研究。分析结果表明，样品在压缩过程中也发生了一个完整的压致相变，此相变在8GPa左右开始，在15GPa左右完成，相变点略低于未掺杂的MgNb_2O_6晶体。这可以解释为Mg~(2+)的电荷比Eu~(3+)的电荷要低，根据电子补偿原理，格点位置Eu~(3+)代替了Mg~(2+)，导致晶格中有Mg~(2+)四面体空位形成。加压过程中MgO_6八面体也由于Eu~(3+)替代空位的存在而使体积改变更容易发生，因此表现为相变点稍微降低。
上述研究结果对深入了解A~(2+)Nb_2O_6的钶铁矿结构在不同压力下的相变过程及高压下的微结构有重要意义,对常压下拉曼峰的归属和指认都有重要的参考价值，为钶铁矿结构材料在微波介电领域的应用提供了实验依据，也为寻找新功能材料提供了方向。
High-pressure and low-temperature research can discover some newphenomenon which substances cannot exhibit at normal pressure androom temperature, disclose new rules and properties, and even find newsubstances. It provides new approaches for investigating substances’properties at high pressure and low temperature and explaining physicalphenomenon at normal pressure and room temperature. With rapiddeveloping of static high pressure measuring technology, diamond anvilcells (DAC) has been widely applied to the high-pressure study of manymaterials. It is well-known that the application of pressure on crystalsresults in decrease of interatomic distance and increase of the overlappingof the adjacent electron orbit，which will change the electronic structureand the forces of the adjacent atoms. Consequently a forced equilibriumstate under pressure is formed. If there are the rearrangement of atomsand the change of symmetry in it, the forced equilibrium state is a newcrystal structure phase, and the phase transition is named as thepressure-induced phase transition. Raman spectroscopy and x-raydiffraction combined with the high-pressure technology can make us convenient to investigate the structural changes of materials underpressure, so the high-pressure in-situ Raman spectroscopy is one of themost useful high-pressure experimental technologies, and supplies asensitive and effective probing method for investigating phase transitionand chemical reaction of the substance in DAC.
Recently, high pressure study on AB2O_6of columbite structure waswidely applied in the production for industrial chemicals and polymers.Raman spectroscopy and x-ray diffraction combined with thehigh-pressure technology can make us convenient to investigate thestructural changes of materials under pressure. At present, high pressurestudy on niobate had been reported, but so far no has accurate transitionpoint or the structural characterization of their high-pressure phase.
Binary niobate ceramies, with the formula A~(2+)Nb_2O_6where A=Ca, Mg,Zn, Fe, Ni, Cd, Co，Mn, have the orthorhombic columbite structure.There is a growing interest in the columbites as microwave dielectricceramics, due to their lower processing temperatures, less complicatedprocessing, the lower cost of niobium compared with tantalum andlow-temperature cofired ceramics (LTCC) with Cu2+.
Up to now, there are few researches on the crystal structural evolutionof columbites under high pressure. Yosuke Shiratori et al. reported onpressure-induced phase transitions in NaNbO_3by high-pressure Ramanspectroscopy, and found different successive transitions below16GPa. Pistorino et al. and Serena et al. reported on crystal structure of (Fe,Mn)(Nb, Ta)2O_6under high pressure by single-crystal X-ray diffraction,and did not observed phase transition below7GPa. On the crystalstructural evolution of A~(2+)Nb_2O_6under high pressure, there have been noreports. The in-situ high pressure Raman spectroscopy is a very powerfultechnology for dynamically investigating the pressure-induced phasetransition of materials, and the in-situ XRD spectrum is intuitive tocharacterize the crystal structure. In the present work, we have performedin-situ high pressure Raman spectroscopy and in-situ XRD measurementswith a DAC to investigate the pressure-induced phase transition inCaNb_2O_6up to23GPa, ZnNb_2O_6and MgNb_2O_6up to30GPa respectively.Besides, the comparison of crystalline phases obtained by high pressureand by low-temperature crystallization is an important direction of highpressure research. We also studied the Raman peaks of these three niobateat low temperature by in-situ Raman spectroscopy associated withLinkam variable-temperature experimental system, in comparison withtheir pressure-induced phase transition.
The main contents and conclusions as follows:
1. Pressure-induced phase transition in CaNb_2O_6.
We have performed the in-situ high pressure studies of CaNb_2O_6using Raman spectroscopy and Synchrotron X-ray diffraction in aDAC up to23GPa. Both Raman and X-ray diffraction data provide evidence of a reversible phase transition from Pbcn to P21/c,beginning from about8GPa and completing at15GPa. Thecompression is mainly on the a direction of stacking ofCaNbNbCaNbNb layers, and the structure expands along the bdirection. The phase transition involves the deformation andrearrangement of the NbO_6and CaO_6octahedra, as well as thedistortion of the NbO_6and CaO_6octahedral chains. Thehigh-pressure phase keeps stable below22.9GPa. All of thesubsequent XRD patterns above15.1GPa are well described withmonoclinic symmetry, and the indexed lattice parameters area=8.2857, b=5.92358, c=4.69152, β=104.41°by the Pawleyrefinements of the X-ray diffraction data.
Temperature dependence Raman spectra of all the crystals showthat there is no phase transition in the whole temperature range(-190-560℃).The temperature-dependent shift of Raman phononsis also discussed in the context.
2. Pressure-induced phase transition in ZnNb_2O_6.
We have performed the in-situ high pressure studies of ZnNb_2O_6using Raman spectroscopy in a DAC up to30GPa. Raman spectraprovide evidence of a reversible phase transition, beginning fromabout10GPa and completing at16GPa. The high-pressure phase keeps stable below20GPa. With the pressure over20GPa, adisordered state formed.
3. Pressure-induced phase transition in MgNb_2O_6.
In situ x-ray diffraction and Raman spectroscopy were used toexplore the pressure-induced phase transformation of MgNb_2O_6single crystal powder with orthorhombic columbite structure29.4GPa and35.0GPa, respectively. Results indicate that MgNb_2O_6initially transforms to the monoclinic structure at about8GPa, andsuch a phase is completed at about15GPa. Also we identified thephase transition as a space group change from Pbcnto P2/C. Thehigh-pressure phase remained stable up to about22.3GPa. With thepressure over22GPa, a disordered state formed.Besides, we carefully studied the crystal structure of1%molEu3+doped MgNb_2O_6under high pressure. A complete phasetransition initially occurred at about8GPa and ultimatelycompleted at around15GPa was observed, which was slightly lessthan pristine MgNb_2O_6. This is reasonably ascribed to higherelectrons deriving from the substitution of Mg2+by Eu3+. Aftersubstitution, the Mg2+tetrahedron vacancy is formed based uponelectronic compensation principle. Furthermore, the volume ofMgO_6octahedraon was also varied by Eu3+substitution and theexistence of vacancy made the phase transition easily happened. As
mentioned above, a slightly decrease of phase transition wasinvestigated in our study.
In summary, our results not only provide an experimental meansfor deeply understanding the phase transition of A~(2+)Nb_2O_6andmicrostructure under different pressure with columbite structurebut also are great significance for its Raman peaks identificationunder normal pressure. Using these experimental methods, it couldbe greatly helpful for the application of columbite structurematerials and novel functional species.
引文
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