本发明属于脉冲激光沉积技术(PLD)以及钙钛矿氧化物薄膜制备领域，具体涉及一种具有良好电输运性能的LaTiO3非晶薄膜及其制备方法。The invention belongs to the field of pulsed laser deposition technology (PLD) and perovskite oxide film preparation, and specifically relates to aLaTiO3 amorphous film with good electrical transport performance and a preparation method thereof.
非晶薄膜的应用在过去几十年中被广泛的研究，由于其较单晶而言制备更加方便，环境要求更为简易，所以会有更宽广的应用前景。但是非晶薄膜通常导电性差，难以做到单晶薄膜那样优良的电输运性。这主要源于非晶薄膜结晶度较差，界面内可以自由移动的电子较少。如何制备出电输运性较好的非晶薄膜是非晶物质研究的一个重要领域。在单晶外延薄膜LaTiO3/SrTiO3中存在着二维电子气已经被证实，在该体系中本该为Mott绝缘体的LaTiO3和能带绝缘体的SrTiO3形成的非晶薄膜反而呈现出金属性，甚至可以作为超导材料。而LaTiO3/SrTiO3的非晶薄膜同样呈现出金属性且有着较为良好的电输运性，这可能是非晶薄膜中同样存在着二维电子气导致的。The application of amorphous films has been widely studied in the past few decades. Compared with single crystals, amorphous films are easier to prepare and have simpler environmental requirements, so they have broader application prospects. However, amorphous films usually have poor conductivity and it is difficult to achieve the same excellent electrical transport properties as single crystal films. This is mainly due to the poor crystallinity of amorphous films and the fewer electrons that can move freely within the interface. How to prepare amorphous films with good electrical transport properties is an important area of research on amorphous materials. It has been confirmed that there is a two-dimensional electron gas in the single crystal epitaxial film LaTiO3 /SrTiO3. In this system, the amorphous film formed by LaTiO3 , which should be a Mott insulator, and SrTiO3 , which is a band insulator, shows metallic properties instead, and can even be used as a superconducting material. The amorphous film of LaTiO3 /SrTiO3 also shows metallic properties and has relatively good electrical transport properties, which may be caused by the existence of two-dimensional electron gas in the amorphous film.
对于非晶 LaTiO3薄膜的界面输运性研究，目前还没有相关的研究。因此，研究非晶 LaTiO3薄膜的界面输运性以及制备出具有良好的电输运性的非晶薄膜是非常有意义的。There is no relevant research on the interface transport properties of amorphous LaTiO3 films. Therefore, it is very meaningful to study the interface transport properties of amorphous LaTiO3 films and to prepare amorphous films with good electrical transport properties.
针对现有技术中存在的不足，本发明提供一种具有良好电输运性能的LaTiO3非晶薄膜及其制备方法。In view of the deficiencies in the prior art, the present invention provides a LaTiO3 amorphous film with good electrical transport performance and a preparation method thereof.
为实现上述目标，本发明所采用的技术方案是：To achieve the above objectives, the technical solution adopted by the present invention is:
一种具有良好电输运性能的LaTiO3非晶薄膜及其制备方法，包括以下步骤：ALaTiO3 amorphous film with good electrical transport performance and a preparation method thereof, comprising the following steps:
（1）将氧化镧和氧化钛前驱体粉末按比例均匀混合后研磨，并用压片机压靶，在马弗炉中高温烧结后得到LaTiO3靶材；(1) The lanthanum oxide and titanium oxide precursor powders are uniformly mixed in proportion and then ground, and a target is pressed using a tablet press, and then sintered at high temperature in a muffle furnace to obtain a LaTiO3 target material;
（2）清洗并刻蚀SrTiO3基片；(2) Cleaning and etching theSrTiO3 substrate;
（3）将LaTiO3靶材和处理后的SrTiO3基片一同放入脉冲激光沉积系统，在合适的条件下生长LaTiO3非晶薄膜；(3) placing the LaTiO3 target and the processed SrTiO3 substrate together in a pulsed laser deposition system to grow a LaTiO3 amorphous film under appropriate conditions;
（4）在真空、室温环境下，获得不同厚度的LaTiO3薄膜。LaTiO3薄膜的电输运性随着厚度的增加而增加，且在厚度达到24nm之后变化趋势逐渐平缓。(4) LaTiO3 films of different thicknesses were obtained under vacuum and room temperature. The electrical transport properties of LaTiO3 films increase with increasing thickness, and the change trend gradually becomes gentle after the thickness reaches 24 nm.
进一步地，步骤（1）中：由于Ti3+的易氧化性，在高温且暴露于空气的环境下烧制LaTiO3陶瓷靶材是只能得到Ti4+的LaTiO3.5相的靶，然而靶材中过量氧的存在对PLD系统而言并不会对生长LaTiO3薄膜产生影响，因为本发明只需要生长LaTiO3薄膜的环境为高真空并且靶材中氧化镧和氧化钛的摩尔比比例为1:2即可，而氧可以通过生长环境进行调节，所以本发明制备了LaTiO3.5相的陶瓷靶材用于生长LaTiO3外延薄膜。首先将氧化镧和氧化钛前驱体粉末按一定比例研磨，时间为30min研磨半小时后向混合粉末中加入10ml无水乙醇，在这个过程中边搅拌边研磨，然后将其放入60℃的干燥箱通风干燥30min得到充分混合的粉末。将干燥后得到的混合粉末研磨2min后先加入10ml无水乙醇搅拌，再次研磨15min并通风等乙醇挥发完全。然后将上述得到的混合粉末放入坩埚并置于马弗炉中升温至1200-1250℃得到镧钛氧粉末。降温后将粉末放入洗净的模具在12Mpa保持10min得到直径1英寸，厚度4mm规格的LaTiO3预烧结靶材。最后将预烧结靶材放入马弗炉在1300-1350℃烧制11-13h即可得到致密的LaTiO3.5陶瓷靶材。Further, in step (1): due to the oxidizability of Ti3+ , firing the LaTiO3 ceramic target at high temperature and exposed to air can only obtain a target of LaTiO3.5 phase with Ti4+ . However, the presence of excess oxygen in the target does not affect the growth of LaTiO3 film for the PLD system, because the present invention only requires a high vacuum environment for the growth of LaTiO3 film and a molar ratio of lanthanum oxide to titanium oxide in the target of 1:2, and oxygen can be adjusted by the growth environment, so the present invention prepares a ceramic target of LaTiO3.5 phase for the growth of LaTiO3 epitaxial film. First, grind the lanthanum oxide and titanium oxide precursor powders in a certain proportion for 30 minutes. After grinding for half an hour, add 10 ml of anhydrous ethanol to the mixed powder, stir and grind during this process, and then put it into a drying oven at 60°C for ventilation and drying for 30 minutes to obtain a fully mixed powder. Grind the mixed powder obtained after drying for 2 minutes, add 10 ml of anhydrous ethanol and stir, grind again for 15 minutes and ventilate until the ethanol evaporates completely. Then put the mixed powder obtained above into a crucible and place it in a muffle furnace and heat it to 1200-1250°C to obtain lanthanum titanium oxide powder. After cooling, put the powder into a clean mold and keep it at 12Mpa for 10 minutes to obtain a LaTiO3 pre-sintered target with a diameter of 1 inch and a thickness of 4mm. Finally, put the pre-sintered target into a muffle furnace and sinter it at 1300-1350°C for 11-13h to obtain a dense LaTiO3.5 ceramic target.
进一步地，步骤（2）中先用丙酮超声清洗5~10min，再用无水乙醇超声清洗5~10min，最后用去离子水清洗5~10min，用氮气吹干后得到清洁表面的STO基片。下面本发明对清洁完的基片进行刻蚀，首先在聚四氟乙烯的烧杯中加入适量的BOE溶液，将STO基片溶液中刻蚀10~15s；然后将基片放入去离子水超声清洗5-10min，除去基片表面残存的BOE溶液；用氮气吹干后得到刻蚀好的STO基片。接着在1000℃恒温退火60min并以同一速率降至室温，得刻蚀好的STO基片。Furthermore, in step (2), first ultrasonically clean the substrate with acetone for 5 to 10 minutes, then ultrasonically clean the substrate with anhydrous ethanol for 5 to 10 minutes, and finally clean the substrate with deionized water for 5 to 10 minutes, and then blow dry the substrate with nitrogen to obtain a STO substrate with a clean surface. The present invention etches the cleaned substrate. First, add an appropriate amount of BOE solution to a polytetrafluoroethylene beaker, and etch the STO substrate in the solution for 10 to 15 seconds; then put the substrate into deionized water for ultrasonic cleaning for 5-10 minutes to remove the BOE solution remaining on the substrate surface; blow dry the substrate with nitrogen to obtain an etched STO substrate. Then, anneal at 1000°C for 60 minutes and cool to room temperature at the same rate to obtain an etched STO substrate.
进一步地，步骤（3）中沉积LaTiO3时，选择沉积温度25-30℃和气压10-6-10-7Torr，在生长过程中，能量密度为1.5J·cm-2。Furthermore, when depositing LaTiO3 in step (3), the deposition temperature is 25-30° C. and the gas pressure is 10−6 -10−7 Torr. During the growth process, the energy density is 1.5 J·cm−2 .
进一步地，步骤（4）先在高真空环境下生长了4nm到32nm的不同厚度下的样品，分别生长了4nm、6nm、8nm、10nm、12nm、16nm、24nm、32nm的LaTiO3薄膜，确定了越高厚度（≥24nm）的LaTiO3薄膜输运性越好。Furthermore, in step (4), samples with different thicknesses ranging from 4 nm to 32 nm were first grown in a high vacuum environment, and LaTiO3 films of 4 nm, 6 nm, 8 nm, 10 nm, 12 nm, 16 nm, 24 nm, and 32 nm were grown respectively. It was determined that the thicker the LaTiO3 film (≥24 nm), the better the transport property.
与现有技术相比，本发明具有以下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明所要解决的技术问题是提供一种具有良好电输运性能的LaTiO3非晶薄膜及其制备方法，与其它制备薄膜技术相比，脉冲激光沉积技术能够制备出高质量的薄膜，使得制备的LaTiO3外延薄膜材料是非晶薄膜，并且具有优良的电输运性，为研究LaTiO3的其他性质提供高质量的薄膜样本。The technical problem to be solved by the present invention is to provide aLaTiO3 amorphous film with good electrical transport properties and a preparation method thereof. Compared with other thin film preparation technologies, pulsed laser deposition technology can prepare high-quality films, so that the preparedLaTiO3 epitaxial thin film material is an amorphous film and has excellent electrical transport properties, providing high-quality thin film samples for studying other properties ofLaTiO3 .
图1为实施例1得到的LaTiO3.5陶瓷靶材XRD谱图；FIG1 is an XRD spectrum of the LaTiO3.5 ceramic target obtained in Example 1;
图2为实施例1不同厚度的非晶LaTiO3薄膜XRR结果图；FIG2 is a graph showing XRR results of amorphous LaTiO3 films of different thicknesses in Example 1;
图3为实施例1 不同厚度的非晶LaTiO3薄膜Ti L-edge的XAS图谱；FIG3 is an XAS spectrum of Ti L-edge of amorphous LaTiO3 films of different thicknesses in Example 1;
图4为实施例1中不同厚度的非晶LaTiO3薄膜R-T曲线图；FIG4 is a RT curve diagram of amorphous LaTiO3 films of different thicknesses in Example 1;
图5为实施例1中300K时薄膜的方块电阻随厚度变化曲线图。FIG. 5 is a curve diagram showing the variation of the sheet resistance of the film with thickness at 300K in Example 1.
下面结合附图对本发明的具体实施方式做详细的说明。The specific implementation modes of the present invention are described in detail below with reference to the accompanying drawings.
在实施例中，所述的具有良好电输运性能的LaTiO3非晶薄膜的制备方法，包括以下步骤：In an embodiment, the method for preparing theLaTiO3 amorphous thin film with good electrical transport properties comprises the following steps:
（1）烧靶：先按照摩尔比1:2的比例将氧化镧和氧化钛混合前驱体粉末混合，放入马弗炉1200-1250℃预烧12h，降温后将粉末放入洗净的模具在12Mpa保持10min得到直径1英寸，厚度4mm规格的LaTiO3预烧结靶材；最后将预烧结靶材放入马弗炉在1300-1350℃烧制11-13h即可得到致密的LaTiO3陶瓷靶材，最后将烧好的靶材用砂纸打磨，得到脉冲激光沉积用的LaTiO3陶瓷；(1) Target sintering: first, mix the lanthanum oxide and titanium oxide mixed precursor powders in a molar ratio of 1:2, put them into a muffle furnace and pre-sinter them at 1200-1250℃ for 12h, and after cooling, put the powder into a clean mold and keep it at 12Mpa for 10min to obtain aLaTiO3 pre-sintered target with a diameter of 1 inch and a thickness of 4mm; finally, put the pre-sintered target into a muffle furnace and sinter it at 1300-1350℃ for 11-13h to obtain a denseLaTiO3 ceramic target, and finally, polish the fired target with sandpaper to obtainLaTiO3 ceramic for pulsed laser deposition;
（2）将SrTiO3基片依次放入丙酮、酒精、去离子水中超声并清洗，时间分别为5min、5min、10min；然后用10:1稀释后的氢氟酸刻蚀基片10-15s，并将刻蚀后的基片在1000℃的管式炉中退火1h；(2) The SrTiO3 substrate was placed in acetone, alcohol, and deionized water for ultrasonic cleaning for 5 min, 5 min, and 10 min, respectively; then the substrate was etched with 10:1 diluted hydrofluoric acid for 10-15 s, and the etched substrate was annealed in a tube furnace at 1000 °C for 1 h;
（3）将LaTiO3靶材和处理后的SrTiO3基片一同放入脉冲激光沉积系统，在合适的条件下在SrTiO3衬底上外延生长出LaTiO3非晶薄膜；(3) placing the LaTiO3 target and the processed SrTiO3 substrate together in a pulsed laser deposition system, and epitaxially growing a LaTiO3 amorphous film on the SrTiO3 substrate under appropriate conditions;
（4）在高真空（10-7Torr）、30℃室温下分别生长了4nm、6nm、8nm、10nm、12nm、16nm、24nm、32nm的不同厚度情况下的LaTiO3非晶薄膜，制备得到了不同厚度的LaTiO3非晶薄膜。(4) LaTiO3 amorphous films with different thicknesses of 4nm, 6nm, 8nm, 10nm, 12nm, 16nm, 24nm, and 32nm were grown under high vacuum (10-7 Torr) and room temperature of30 °C.
下面通过更具体实施例加以说明。The following is explained with more specific examples.
实施例1Example 1
一种具有良好电输运性能的非晶薄膜的制备方法，包括以下步骤：A method for preparing an amorphous film with good electrical transport properties comprises the following steps:
（1）先按照1:2将氧化镧和氧化钛混合，放入马弗炉1200-1250℃预烧12h，降温后将粉末放入洗净的模具在12Mpa保持10min得到直径1英寸，厚度4mm规格的LaTiO3预烧结靶材；最后将预烧结靶材放入马弗炉在1300-1350℃烧制12h即可得到致密的LaTiO3陶瓷靶材，最后将烧好的靶材用砂纸打磨，得到脉冲激光沉积用的LaTiO3陶瓷；(1) First, lanthanum oxide and titanium oxide are mixed in a ratio of 1:2, and pre-sintered in a muffle furnace at 1200-1250°C for 12 hours. After cooling, the powder is placed in a clean mold and kept at 12Mpa for 10 minutes to obtain aLaTiO3 pre-sintered target with a diameter of 1 inch and a thickness of 4 mm; finally, the pre-sintered target is placed in a muffle furnace and fired at 1300-1350°C for 12 hours to obtain a denseLaTiO3 ceramic target. Finally, the fired target is polished with sandpaper to obtainLaTiO3 ceramics for pulsed laser deposition;
（2）将SrTiO3基片依次放入丙酮、酒精、去离子水中清洗，清洗时间分别为5min、5min、10min；然后用10:1稀释后的氢氟酸刻蚀基片12s，并在1000℃的管式炉中退火1h；(2) The SrTiO3 substrate was cleaned in acetone, alcohol, and deionized water in turn for 5 min, 5 min, and 10 min, respectively; the substrate was then etched with 10:1 diluted hydrofluoric acid for 12 s and annealed in a tube furnace at 1000 °C for 1 h;
（3）将LaTiO3靶材和处理后的SrTiO3基片一同放入脉冲激光沉积系统，在SrTiO3基片上生长出LaTiO3非晶薄膜；沉积LaTiO3温度为30℃，气压为10-7torr，能量密度为1.5 J·cm-2。(3) The LaTiO3 target and the processed SrTiO3 substrate were placed in a pulsed laser deposition system to grow a LaTiO3 amorphous film on the SrTiO3 substrate; the LaTiO3 deposition temperature was 30°C, the gas pressure was 10-7 torr, and the energy density was 1.5 J·cm-2 .
（4）在高真空(10-7Torr), 能量密度为1.5 J·cm-2下，分别生长了4nm、6nm、8nm、10nm、12nm、16nm、24nm、32nm的不同厚度下的LaTiO3薄膜。(4) Under high vacuum (10-7 Torr) and an energy density of 1.5 J·cm-2 , LaTiO3 films with different thicknesses of 4nm, 6nm, 8nm, 10nm, 12nm, 16nm, 24nm, and 32nm were grown.
对不同厚度的LaTiO3非晶薄膜进行电运输性能测试，采用的是4200-SCS系统，采用超声波点焊机连接引线，测试了LaTiO3薄膜的电阻曲线，探索了薄膜和衬底之间二维电子气的影响。The electrical transport performance ofLaTiO3 amorphous films of different thicknesses was tested using a 4200-SCS system. The leads were connected using an ultrasonic spot welder, the resistance curve of theLaTiO3 film was tested, and the influence of the two-dimensional electron gas between the film and the substrate was explored.
测电阻是主要是使用四探针法测试了薄膜电阻率，用wire bonder设备薄膜连接好引脚，在连接的过程中注意过长的引线需要避免与其他引脚或低温腔内胆其他部位接触，防止接线断路；安装好低温腔样品架外壳后，需检查是否漏气，保证低温腔内的真空度，使测试数据可靠准确。The resistance measurement mainly uses the four-probe method to test the film resistivity. The pins are connected with the thin film using a wire bonder device. During the connection process, it is necessary to avoid contact between the long leads and other pins or other parts of the cryogenic chamber to prevent the wiring from being broken. After installing the cryogenic chamber sample holder shell, it is necessary to check for leaks to ensure the vacuum degree in the cryogenic chamber so that the test data is reliable and accurate.
试验例Test example
采用粉晶XRD对实施例1所制备的LaTiO3.5靶材，通过图1的LaTiO3.5陶瓷靶材的XRD结果与LaTiO3.5标准卡片PDF#42-0517对比可以确定所烧制的LaTiO3.5陶瓷靶材中没有其他相的衍射峰出现，并且在XRD谱图中，衍射峰强度高，衍射峰尖锐且半高宽较小，这表明所制备的LaTiO3.5靶材结晶性非常好，可用于PLD系统进行LaTiO3薄膜的外延生长。Powder XRD was used to analyze the LaTiO3.5 target prepared in Example 1. By comparing the XRD results of the LaTiO3.5 ceramic target in Figure 1 with the LaTiO3.5 standard card PDF#42-0517, it can be determined that no diffraction peaks of other phases appear in the fired LaTiO3.5 ceramic target, and in the XRD spectrum, the diffraction peak intensity is high, the diffraction peak is sharp and the half-width is small, which indicates that the prepared LaTiO3.5 target has very good crystallinity and can be used for the epitaxial growth of LaTiO3 thin films in the PLD system.
图2为了准确测得不同厚度LaTiO3非晶薄膜的厚度，本发明对上述LaTiO3非晶薄膜的8个不同厚度（LTO-4nm、6nm、8nm、10nm、12nm、16nm、24nm、32nm）的薄膜进行了非晶XRR表征，得到如下图2所示结果。通过XRR结果可以看到不同厚度非晶LaTiO3薄膜的振荡周期以及厚度。Figure 2 In order to accurately measure the thickness of LaTiO3 amorphous films of different thicknesses, the present invention performs amorphous XRR characterization on8 films of different thicknesses (LTO-4nm, 6nm, 8nm, 10nm, 12nm, 16nm, 24nm, 32nm) of the above-mentioned LaTiO 3 amorphous films, and obtains the results shown in Figure 2. The XRR results show the oscillation period and thickness of amorphous LaTiO3 films of different thicknesses.
图3为不同厚度的非晶LaTiO3薄膜Ti L-edge的XAS图谱的研究可以发现，三个不同厚度的非晶 LaTiO3薄膜（LTO-4nm、8nm、32nm）的L3eg峰对应结合能都为459.6eV，L2eg峰对应结合能同样都是465eV，说明非晶 LaTiO3薄膜中的Ti均为+3价，是完全没有结晶的LaTi3+O3薄膜。Figure 3 shows the XAS spectrum of Ti L-edge of amorphousLaTiO3 films of different thicknesses. It can be found that the corresponding binding energy of theL3eg peak of three amorphousLaTiO3 films of different thicknesses (LTO-4nm, 8nm, 32nm) is 459.6eV, and the corresponding binding energy of theL2eg peak is also 465eV, indicating that the Ti in the amorphousLaTiO3 film is +3 valence, and it is a LaTi3+O3 film without crystallization.
图4为不同厚度（LTO-4nm、6nm、8nm、10nm、12nm、16nm、24nm、32nm）LaTiO3薄膜的R-T曲线图，从图中可以看到，随着测试温度的降低，薄膜与衬底界面处的导电性增强，呈现出金属特性，且越厚的薄膜导电性越强。Figure 4 is the RT curve of LaTiO3 films of different thicknesses (LTO-4nm, 6nm, 8nm, 10nm, 12nm, 16nm, 24nm, 32nm). It can be seen from the figure that as the test temperature decreases, the conductivity at the interface between the film and the substrate increases, showing metallic properties, and the thicker the film, the stronger the conductivity.
图5为300K时薄膜的方块电阻随厚度的变化曲线，从图中结果可以看到，随着薄膜厚度的升高，薄膜的方块电阻逐渐变小。通过曲线发现，方块电阻阻值在达到24nm之后下降趋势逐渐趋于平稳。Figure 5 is a curve showing the change of sheet resistance of the film with thickness at 300K. From the results in the figure, we can see that as the thickness of the film increases, the sheet resistance of the film gradually decreases. The curve shows that the downward trend of the sheet resistance gradually stabilizes after reaching 24nm.
综上所述，本发明认为在高真空、室温条件下，LaTiO3薄膜的电输运性随着厚度的增加而增加，且在厚度达到24nm之后下降趋势逐渐平缓。In summary, the present invention believes that under high vacuum and room temperature conditions, the electrical transport property of LaTiO3 thin film increases with increasing thickness, and the downward trend gradually slows down after the thickness reaches 24 nm.
以上详细描述了本发明的较佳具体实施例。应当理解，本领域的普通技术无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此，凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案，皆应在由权利要求书所确定的保护范围内。The preferred specific embodiments of the present invention are described in detail above. It should be understood that ordinary technicians in the field can make many modifications and changes based on the concept of the present invention without creative work. Therefore, all technical solutions that can be obtained by technicians in the technical field based on the concept of the present invention through logical analysis, reasoning or limited experiments on the basis of the prior art should be within the scope of protection determined by the claims.
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| CN202211438775.8 | 2022-11-17 | ||
| CN202211438775.8ACN115652258A (en) | 2022-11-17 | 2022-11-17 | Amorphous thin film with good electrical transport properties and preparation method thereof |
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| WO2024103777A1true WO2024103777A1 (en) | 2024-05-23 |
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| PCT/CN2023/104473CeasedWO2024103777A1 (en) | 2022-11-17 | 2023-06-30 | Amorphous thin film with good electrical transport performance and preparation method therefor |
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