Name: tuning oxide properties by oxygen vacancy control during growth and annealing
Uploaded: 2023-06-09T15:00:00
Description: Watch this Scientific Journal Video about Tuning Oxide Properties by Oxygen Vacancy Control During Growth and Annealing at JoVE.com

作者感谢丹麦技术大学的J. Geyti提供的技术援助。F. Trier感谢VILLUM FONDEN的研究资助VKR023371（SPINOX）的支持。D. V. Christensen感谢诺和诺德基金会NERD计划的支持：新的探索性研究和发现，高级资助NNF21OC0068015。

1. 通过不同的生长条件控制性能
<ol><li>制备高质量表面的SrTiO3
	<ol><li>购买混合端接的 SrTiO3 衬底（例如，尺寸为 5 mm x 5 mm x 0.5 mm），相对于 （001） 晶平面的典型表面角度为 0.05°–0.2°。 注意： 错切角度决定了表面的平整度，这对于基板上的外延生长以及界面处产生的特性非常重要。</li>
		<li>通过在标准超声仪中在丙酮中超声处理5分钟和乙醇在室温下超声处理5?...

<ol>
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这里描述的方法依赖于使用氧含量来控制氧化物特性，因此氧分压和工作温度是关键参数。如果系统的总氧化状态以系统与周围大气保持热力学平衡的方式进行调整（即在高温下pO2 发生变化），则这些变化是可逆的。然而，在基于SrTiO3的异质结构的情况下，界面氧空位通常使用脉冲激光沉积形成，其可以捕获非平衡状态的氧化态34。在这种情况下，沉积时和之后...

氧含量在氧化物材料的性能中起着至关重要的作用。氧具有很高的电负性，并且在全离子极限下，从相邻阳离子吸引两个电子。当形成氧空位时，这些电子被捐赠给晶格。电子可以被捕获并形成局部状态，或者它们可以离域并能够传导充电电流。局部状态通常位于价带和导带之间的带隙中，总角动量可以是非零1，2，3。因此，局部状态可以形成局部磁矩，并对例如光学和磁性产生很大影响1，2，3。如果电子离域，它们有助于流动电荷载流子的密度。此外，如果形成氧空位或其他缺陷，晶格会适应缺陷。因此，缺陷的存在自然会导致局部应变场、对称性破坏以及氧化物中电子和离子传输的修饰。
因此，控制氧化学计量通常是调整氧化物材料的光学、磁性和传输特性的关键。一个突出的例子是SrTiO 3和SrTiO3基异质结构，其中材料系统的基态对氧含量非常敏感。未掺杂的SrTiO 3是一种非磁性绝缘体，带隙为3.2 eV;然而，通过引入氧空位，SrTiO3将状态从绝缘变为金属导电，在2 K4时电子迁移率超过10，000 cm2 / Vs。在低温（T < 450 mK）下，超导性甚至可能是青睐的基态5，6。还发现SrTiO3中的氧空位使其成为铁磁7，并导致可见光谱中的光学跃迁从透明到不透明2。十多年来，人们一直对在SrTiO 3上沉积各种氧化物（例如LaAlO 3，CaZrO 3和γ-Al2O 3）并检查界面8，9，10，11，12，13上产生的特性非常感兴趣。.在某些情况下，事实证明界面的属性与在母材料中观察到的属性明显不同。基于SrTiO3的异质结构的一个重要结果是电子可以限制在界面中，这使得使用静电门控控制与流动电子密度相关的性质成为可能。通过这种方式，可以使用电场来调整例如界面的电子迁移率14，15，超导11，电子对16和磁性状态17。
界面的形成还可以控制SrTiO 3化学，其中顶部薄膜在SrTiO3上的沉积可用于诱导界面18，19上的氧化还原反应。如果在SrTiO 3上沉积具有高氧亲和力的氧化膜，氧气可以从SrTiO 3的近表面部分转移到顶部薄膜，从而减少SrTiO3并氧化顶部薄膜（见图1）。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/58737/58737fig01v2.jpg"> 图 1：SrTiO3 中的氧空位形成。 在沉积具有高氧亲和力的薄膜期间，如何在SrTiO 3 的界面附近区域形成氧空位和电子的示意图。经Chen等人研究许可转载图18。版权所有 2011 美国化学学会。 <a href="https://www.jove.com/files/ftp_upload/58737/58737fig1large.jpg" target="_blank">请点击此处查看此图的大图。</a>
在这种情况下，氧空位和电子在界面附近形成。该过程有望成为在SrTiO 3与室温生长的金属薄膜或氧化物（如无定形LaAlO 3 18，20或γ-Al2O310，21，22，23）界面处沉积期间形成的导电性的来源。因此，这些基于SrTiO3的界面的性质对界面处的氧含量高度敏感。
在这里，我们报告了使用沉积后退火和脉冲激光沉积参数的变化，通过调整氧含量来控制氧化物材料中的性能。我们使用室温下沉积在SrTiO 3上的γ-Al2O 3或无定形LaAlO 3作为示例，说明如何通过控制氧空位的数量将载流子密度，电子迁移率和薄层电阻改变几个数量级。这些方法提供了一些超出静电门控获得的好处，静电门控通常用于调整电气9，11，14，在某些情况下用于调节磁性15，17特性。这些好处包括形成（准）稳定的最终状态和避免使用电场，这需要与样品电接触并可能引起副作用。
在下文中，我们将回顾通过控制氧含量来调整氧化物性质的一般方法。这通过两种方式完成，即1）通过在合成氧化物材料时改变生长条件，以及2）通过在氧气中退火氧化物材料。这些方法可用于调整许多氧化物和一些一氧化碳材料中的一系列特性。我们提供了一个具体的例子来调整SrTiO3基异质结构界面处的载流子密度。确保保持高水平的清洁度以避免样品污染（例如，使用手套、专用于 SrTiO3 的管式炉和非磁性/耐酸镊子）。

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		<tr height="21">
			<td height="21" style="height:21px;width:216px;">SrTiO3</td>
			<td style="width:264px;">Crystec</td>
			<td style="width:264px;"></td>
			<td style="width:516px;">Single crystalline (001) oriented, 0.05-0.2 degree miscut angle</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">LaAlO3</td>
			<td style="width:264px;">Shanghai Daheng Optics and Fine Mechanics Co.Ltd.</td>
			<td style="width:264px;"></td>
			<td>Single crystalline</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Al2O3</td>
			<td style="width:264px;">Shanghai Daheng Optics and Fine Mechanics Co.Ltd.</td>
			<td style="width:264px;"></td>
			<td>Single crystalline</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Chemicals and gases</td>
			<td style="width:264px;">Standard suppliers</td>
			<td style="width:264px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Silver paste</td>
			<td style="width:264px;">SPI Supplies, Structure Probe Inc</td>
			<td style="width:264px;"></td>
			<td>05001-AB, High purity silver paint</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Ultrasonicator</td>
			<td style="width:264px;">VWR</td>
			<td style="width:264px;"></td>
			<td>USC500D HF45kHz/100W</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Wedge wire bonder</td>
			<td style="width:264px;">Shenzhen Baixiangyuan Science &#38; Technology Co.,Ltd.</td>
			<td style="width:264px;"></td>
			<td>HS-853A Aluminum wire bonder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Pulsed laser deposition</td>
			<td style="width:264px;">Twente Solid State Technologies (TSST)</td>
			<td style="width:264px;"></td>
			<td style="width:516px;">PLD from TSST with software version V3.0.29, equipped with a 248 nm KrF 
			nanosecond laser (Compex Pro 205 F) from Coherent</td>
		</tr>
		<tr height="105">
			<td height="105" style="height:105px;width:216px;">Resistance measurement setup</td>
			<td style="width:264px;">Custom made</td>
			<td style="width:264px;"></td>
			<td style="width:516px;">Based on the following electrical instruments and custom written software: 
			Keithley 6221 DC and AC current source 
			Keithley 2182A nanovoltmeter 
			Keithley 7001 switch system with a matrix card 
			Keithley 6487 picoammeter</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:216px;">Hall measurements</td>
			<td style="width:264px;">Cryogenics</td>
			<td style="width:264px;"></td>
			<td style="width:516px;">Based on the following electrical instruments and custom written software: 
			Keithley 2400 DC current source 
			Keithley 2182A nanovoltmeter 
			Keithley 7001 switch system with a matrix card</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Furnace</td>
			<td style="width:264px;">Custom made</td>
			<td style="width:264px;"></td>
			<td style="width:516px;">Custom written software control of a FTTF 500/70 tube furnace from Scandia Ovnen AS and a eurotherm 2216e temperature controller</td>
		</tr>
	</tbody>
</table>

tuning oxide properties by oxygen vacancy control during growth and annealing

氧化物材料的电学、光学和磁性通常可以通过改变氧含量来控制。在这里，我们概述了两种改变氧含量的方法，并提供了调整SrTiO3基异质结构的电性能的具体示例。在第一种方法中，通过在脉冲激光沉积过程中改变沉积参数来控制氧含量。在第二种方法中，通过在薄膜生长后使样品在高温下在氧气中退火来调整氧含量。这些方法可用于各种氧化物和非氧化物材料，其中其性质对氧化态的变化很敏感。
这些方法与静电门控有很大不同，静电门控通常用于改变受限电子系统的电子特性，例如在基于SrTiO 3的异质结构中观察到的电子特性。通过控制氧空位浓度，我们能够将载流子密度控制在许多数量级上，即使在非受限电子系统中也是如此。此外，可以控制对流动电子密度不敏感的特性。

通过不同的生长条件控制属性 在氧化物沉积过程中改变沉积参数会导致性能发生较大变化，特别是对于基于SrTiO3的异质结构，如图 2所示。
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/58737/58737fig2v2.jpg"> 图 2：通过调整顶层厚度来控制传输属性。（a） γ-...

Watch this Scientific Journal Video about Tuning Oxide Properties by Oxygen Vacancy Control During Growth and Annealing at JoVE.com

Tuning Oxide Properties by Oxygen Vacancy Control During Growth and Annealing

氧化物材料显示出许多奇特的特性，可以通过调节氧含量来控制。在这里，我们演示了通过改变脉冲激光沉积参数和执行后退火来调整氧化物中的氧含量。例如，SrTiO3基异质结构的电子性能通过生长修饰和退火来调节。

通过生长和退火过程中的氧空位控制来调整氧化物性能

Electrical, optical, and magnetic properties of oxide materials can often be controlled by varying the oxygen content. Here we outline two approaches for ...

这里介绍的方法允许在沉积期间和之后控制氧化物薄膜中的氧空位量。这种方法的主要优点是可以通过修改氧空位的数量来调整电和磁特性。氧空位在大多数氧化物材料中都是功能缺陷，因此许多氧化物的性质可以通过使用这种方法的缺陷工程系统地控制。演示该程序的将是Shinhee，Carlos和Eric，我们实验室的博士后和两名博士生。首先，购买混合封端钛酸锶衬底，其典型表面角度相对于晶面为0.05至0.2度。通过在丙酮中超声处理五分钟清洁所需数量的底物。然后在70摄氏度的清水中超声处理底物20分钟，使氧化锶溶解或在以氧化锶终止的表面域形成氢氧化锶配合物，同时保持化学稳定的二氧化钛终止域不变。同时，通过将盐酸缓慢加入水中，然后将硝酸加入溶液中来制备王水溶液。接下来，在含有盐酸，硝酸和水的酸性溶液中，在通风橱中超声处理底物20分钟，以选择性地蚀刻氧化锶由于氧化锶表面结构域的基本性质，二氧化钛的酸度以及氢氧化锶配合物的存在。通过在100毫升清水中超声处理在通风橱中室温下五分钟，从底物中除去残留的酸。然后将基材在一格氧气的气氛中以每小时100摄氏度的加热和冷却速度在陶瓷管式炉中烘烤1小时，以将基材表面放松到低能量状态。要在基板上沉积薄膜，请将基板安装在加热器或芯片载体上，具体取决于在沉积过程中是否要执行NC2传输测量。接下来，将二氧化钛封端的基板放置在距离单晶氧化铝靶材 4.7 厘米处，以便在室温下将 γ 氧化铝典型沉积在钛酸锶上。准备在 10 的氧气压力下从单个结晶氧化铝靶材烧蚀到功率负 5 毫巴。通过使用 10 到功率负 6 到 0.1 毫巴的氧气沉积压力，或通过改变其他沉积参数，使用氧含量来调整属性。孵育后，观察基底中所需厚度的γ氧化铝沉积。接下来，从沉积室中取出样品，并停止任何电气测量。然后将样品储存在真空中。在真空或氮气中储存时，样品降解最慢。使用银浆将样品安装在芯片载体上。然后使用范德堡几何形状中铝线的楔形引线键合将样品电连接到芯片载体。接下来，将芯片载体与样品一起放入密闭炉中。然后使用具有耐热绝缘的连接器和电线，将芯片载体电连接到测量设备，并开始薄层电阻测量。然后将装有样品的芯片载体放入密闭炉中，用用于退火的气体彻底冲洗，同时检查样品电阻是否对气氛变化敏感。使用所需的退火曲线对样品进行退火，具体取决于顶膜的厚度和所需的氧掺入速率。当薄层电阻发生所需变化时中止退火。使用这种设置，可以在脉冲激光沉积过程中原位监测氧化铝钛酸锶和铝酸镧钛酸镧等氧化物异质结构中薄层电阻的发展。当通过非原位测量或通过原位氧气冲洗改变测量环境时，可以观察到钛酸锶基异质结构的薄层电阻的显着变化。在伽马氧化铝沉积在钛酸锶上的样品中，电子迁移率在室温下基本保持不变，但当沉积压力变化时，在两个开尔文处发生显着变化。氧化物异质结构的性质也可以在使用退火沉积后进行调整。最终状态由退火时间和退火温度和气氛决定。在不同的退火温度下测量由伽马氧化铝或无定形镧铝酸盐组成的异质结构的片状导电剂。观察到非晶态铝酸镧钛酸锶异质结构的电导下降最快。对于钛酸锶异质结构，通过控制退火和氧气来控制载流子密度。连续的退火步骤导致载流子密度的稳定降低，并从金属导电体过渡到绝缘界面。改变钛酸锶异质结构中的导电状态可以实现不同的性能。在这里，在退火之前不可能尝试使用导电原子力显微镜写入纳米线。但是，退火后，可以在界面处写入和擦除导电线。使用这种方法，我们可以系统地改变氧化物异质结构的磁性和电子性质，并以这种方式研究氧空位在确定这些性质中的作用。

Research

JoVE Journal

Chemistry

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

原子定义模板复合氧化物薄膜的外延生长

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

科研

化学

Tuning a Parallel Segmented Flow Column and Enabling Multiplexed Detection

调优并行分段流动列和启用多重检测

Active flow technology (AFT) is new form of column technology that was designed to overcome flow heterogeneity to increase separation performance in terms ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

铱氧化物纳米颗粒对硒化镉硫化镉@纳米棒光化学氧化增长

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

二氧化钛<sub&gt; 2</sub与由软化学法合成的超疏水性和高IR反射属性&gt;涂覆的空心玻璃微球

This manuscript proposes a soft-chemistry method to develop superhydrophobic and highly IR-reflective hollow glass microspheres (HGM). The anatase TiO2 ...

Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods

金属氧化物结构的气溶胶辅助化学气相沉积: 氧化锌棒

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, ...

Fabrication of Spherical and Worm-shaped Micellar Nanocrystals by Combining Electrospray, Self-assembly, and Solvent-based Structure Control

结合电喷雾、自组装和溶剂型结构控制制备球形和蜗杆状胶束纳米晶

Micellar nanocrystals (micelles with encapsulated nanocrystals) have become an emerging major class of nanobiomaterials. We describe a method of ...

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

Syntheses, Crystallization, and Spectroscopic Characterization of 3,5-Lutidine N-Oxide Dehydrate

35-吡啶N-氧化物脱水的合成、结晶和光谱表征

The synthesis of 3,5-lutidine N-oxide dehydrate, 1, was achieved in the synthesis route of 2-amino-pyridine-3,5-dicarboxylic acid. Ochiai first used the ...

Surface Properties of Synthesized Nanoporous Carbon and Silica Matrices

合成纳米碳和二氧化硅矩阵的表面性能

In this work, we report the synthesis and characterization of ordered nanoporous carbon material (also called ordered mesoporous carbon material [OMC]) ...

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

复合金属氧化物纳米粒子的熔融盐合成

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. ...

U2O5 Film Preparation via UO2 Deposition by Direct Current Sputtering and Successive Oxidation and Reduction with Atomic Oxygen and Atomic Hydrogen

U2O5 Film Preparation via UO2 Deposition by Direct Current Sputtering and Successive Oxidation and Reduction with Atomic Oxygen and Atomic Hydrogen

利用uo2沉积制备 u2o5 薄膜, 利用原子氧和原子氢连续氧化还原

We describe a method to produce U2O5 films in situ using the Labstation, a modular machine developed at JRC Karlsruhe. The Labstation, an essential part ...