CN110739221B - 带隙可调的锡氧化物薄膜制备方法 - Google Patents
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000137 annealing Methods 0.000 claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical group O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 230000003287 optical effect Effects 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 30
- 239000010409 thin film Substances 0.000 description 9
- 238000012512 characterization method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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Abstract
带隙可调的锡氧化物薄膜制备方法，本发明涉及光电探测技术领域，具体涉及一种带隙可调的锡氧化物薄膜制备方法。锡氧化物薄膜制备方法，包括湿法清洗、射频磁控溅射、退火步骤。本发明的方法，通过控制氧分压和退火，形成一种混合相锡氧化物薄膜材料，改变了锡氧化物薄膜的结构，对光学带隙进行调制，实现了光学吸收的波段涵盖UVA,UVB,UVC，可实现制备紫外多波段的探测器。
Description
技术领域
本发明涉及光电探测技术领域，具体涉及一种带隙可调的锡氧化物薄膜制备方法。
背景技术
人眼不识别电磁波谱中的紫外光波段，需要制备光电探测器应用于军事勘查、火情探测、臭氧监测、化学分析等领域中。但紫外光的光子能量相对较高，所以制备紫外探测器的材料多为宽禁带半导体。常见的材料体系有ZnO、Ga2O3、SiC、GaN、MgO等。随着该领域的速发展，新型光电探测材料不断地涌现，如氧化亚锡(SnO)和氧化锡(SnO2)。SnO作为P型半导体材料，直接带隙为2.7eV。SnO具有p型导电特性的主要原因是锡空位的存在以及氧化态的Sn2+占据了氧原子的间隙位置，SnO的氧的2p能级与锡的5s能级都位于价带最大值(VBM)附近，所以能级较为接近易于轨道杂化，进而使空穴迁移率增强，这也正是p型金属氧化物稀缺的原因。作为元素组成相同但比例不同的氧化锡(SnO2)是典型的n型金属氧化物半导体材料，直接带隙为3.6eV，具有优异的性能，被广泛应用于光电探测器,催化,气体传感器，储能,太阳能电池等领域。但是，目前还未有带隙可调的锡氧化物薄膜技术的记载。
当前记载的锡氧化物的制备方法,主要有静电纺丝法、脉冲激光沉积法、水热法、分子束外延法、磁控溅射法等。与其他方法相比,磁控溅射法具有操作简单、均匀性好、实验重复性高等优点，因此本发明将选用该方法实现锡氧化物薄膜的制备，以优化锡氧化物薄膜光电性能，实现带隙可调的锡氧化物薄膜的制备。
发明内容
本发明的目的在于提供一种锡氧化物薄膜制备方法，通过控制氧分压和退火过程，来有效地调制锡氧化物薄膜的带隙，从而优化锡氧化物薄膜光电性能。
本发明带隙可调的锡氧化物薄膜制备方法，包括湿法清洗、射频磁控溅射、退火步骤，其特征在于具体步骤包括：
S1，湿法清洗衬底，使衬底干净，干燥；
S2，射频磁控溅射，将衬底放入磁控溅射设备中，在设备真空度到达6.0×10-4pa以下时，分别在8％、10％、0％的氧分压下，进行溅射薄膜；
其中，氧分压＝氧气气体流量/氧气和氩气总气体流量；
S3，退火，退火在大气气氛下进行，退火温度为250-300℃，退火时间为30-60min。
本发明的方法，通过控制氧分压，选择8％、10％、0％的氧分压和退火，形成一种混合相锡氧化物薄膜材料，改变了锡氧化物薄膜的结构，对光学带隙进行调制，实现了光学吸收的波段涵盖UVA,UVB,UVC，可实现制备紫外多波段的探测器。在其他氧分压下也能实现锡氧化物薄膜的制备，但是对光学带隙的调控作用不大。并不能实现对对紫外波段有响应。
本发明的锡氧化物薄膜制备方法，制备温度较低，实现了低能耗制备锡氧化物薄膜。制备过程简便，操作可行，制备得到的锡氧化物薄膜具有优异的光电性能。
附图说明
图1为制得的锡氧化物薄的膜XRD图；
A、B、C分别代表8％、10％、0％的氧分压。
图2为实施例1制得的锡氧化物薄膜的TEM图。
图3为实施例1制得的锡氧化物薄膜退火前的AFM图。
图4为实施例1制得的锡氧化物薄膜退火后的AFM图。
图5为制得的锡氧化物薄膜的光学带隙图。
具体实施方式
实施例1：锡氧化物薄膜制备方法，包括湿法清洗、射频磁控溅射、退火步骤，具体步骤如下：
S1，湿法清洗,将衬底放入双氧水、氨水、去离子水按1:1:3体积比配比的混合溶液中，在80℃温度下，恒温加热30min，用去离子水清洗，吹干。
S2，射频磁控溅射，将经处理的衬底放入磁控溅射的样品托上，在设备真空度到达6.0×10-4pa以下时，调节氧分压为10％，设置启辉压强0.6pa和120W溅射功率,溅射40min。
S3，退火，采用管式炉在大气气氛下进行退火，退火温度300℃，退火时间1h，直至样品降到室温，获得锡氧化物薄膜,按质量混合相的氧化锡：氧化亚锡为3：7。
对获得的锡氧化物薄膜进行表征分析。
如图1所示，为不同氧分压下锡氧化物的X射线衍射成像图，可看到薄膜是氧化锡和氧化亚锡的混合相，并且随着氧分压的增大氧化锡的含量会有所增加。
如图2所示，为锡氧化物薄膜的透射电镜成像图，可看到氧化锡及氧化亚锡的晶格条纹。
如图3所示，为锡氧化物薄膜退火前的原子力显微镜表征图，可看到薄膜表面较均匀，呈现颗粒状。
如图4所示，为锡氧化物薄膜退火后的原子力显微镜表征图，可看到薄膜表面粗糙度并无明显变化。
如图5所示，为锡氧化物薄膜的光学带隙图，如图5中1、2、3，分别对应于氧分压0％、8％、10％，通过将(αhν)2与hν图的线性部分拟合得到薄膜的光学带隙，发现样品退火后带隙值Eg会增大，并且也会随着氧分压的增大而增大，带隙可调的范围是2.16-3.96eV。
实施例2：锡氧化物薄膜制备方法，包括湿法清洗、射频磁控溅射、退火步骤，除调节氧分压为8％外，其它具体步骤和参数同实施例1，获得锡氧化物薄膜,按质量混合相的氧化锡：氧化亚锡为1：4。
实施例3：锡氧化物薄膜制备方法，包括湿法清洗、射频磁控溅射、退火步骤，除调节氧分压为0％外，其它具体步骤和参数同实施例1。获得锡氧化物薄膜,按质量混合相的氧化锡：氧化亚锡为0：1。
本发明提到的实例仅用于说明本发明的可行性，而不是仅仅限制本发明的范围。除此之外，在无实质性改变实验制备技术的情况下，亦当视为本发明的可实施范畴。
Claims (1)
1.带隙可调的锡氧化物薄膜制备方法，包括湿法清洗、射频磁控溅射、退火步骤，其特征在于具体步骤包括：
S1，湿法清洗，将衬底放入双氧水、氨水、去离子水按1:1:3体积比配比的混合溶液中，在80℃温度下，恒温加热30min，用去离子水清洗，吹干；
S2，射频磁控溅射，将衬底放入磁控溅射设备中，在设备真空度到达6.0×10-4 pa以下时，分别在8%、10%的氧分压下，进行溅射薄膜；
其中，氧分压=氧气气体流量/氧气和氩气总气体流量；
S3，退火，退火在大气气氛下进行，退火温度为250-300℃，退火时间为30-60 min；
10%的氧分压下，获得锡氧化物薄膜,按质量混合相的氧化锡：氧化亚锡为3：7；
8%的氧分压下，获得锡氧化物薄膜,按质量混合相的氧化锡：氧化亚锡为1：4。
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