CN103943700A - InGaAsN thin film grown on GaAs substrate and manufacturing method of InGaAsN thin film - Google Patents
InGaAsN thin film grown on GaAs substrate and manufacturing method of InGaAsN thin film Download PDFInfo
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- 229910001218 Gallium arsenide Inorganic materials 0.000 title claims abstract description 125
- 239000000758 substrate Substances 0.000 title claims abstract description 90
- 239000010409 thin film Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 8
- 239000010408 film Substances 0.000 claims description 32
- 238000007872 degassing Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 229910052785 arsenic Inorganic materials 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052733 gallium Inorganic materials 0.000 claims description 8
- 239000005416 organic matter Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
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- 229910021641 deionized water Inorganic materials 0.000 claims description 4
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- 238000005070 sampling Methods 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
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- 239000000463 material Substances 0.000 description 19
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- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000013082 photovoltaic technology Methods 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003887 surface segregation Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- H10F77/1248—Active materials comprising only Group III-V materials, e.g. GaAs having three or more elements, e.g. GaAlAs, InGaAs or InGaAsP
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Abstract
本发明公开了一种生长在GaAs衬底上的InGaAsN薄膜，包括生长在GaAs衬底上的GaAs缓冲层、生长在GaAs缓冲层上的InGaAsN外延层薄膜。本发明还公开上述生长在GaAs衬底上的InGaAsN薄膜的制备方法，GaAs缓冲层和InGaAsN外延层薄膜均采用分子束外延生长方法。本发明得到的InGaAsN薄膜表面平整、成分均匀，带宽为1eV，对半导体器件领域，尤其是太阳电池领域，有着积极的促进意义。
The invention discloses an InGaAsN thin film grown on a GaAs substrate, comprising a GaAs buffer layer grown on the GaAs substrate and an InGaAsN epitaxial layer thin film grown on the GaAs buffer layer. The invention also discloses the preparation method of the above-mentioned InGaAsN thin film grown on the GaAs substrate, and the GaAs buffer layer and the InGaAsN epitaxial layer thin film both adopt the molecular beam epitaxy growth method. The InGaAsN thin film obtained by the invention has smooth surface, uniform composition and 1eV bandwidth, and has positive promotion significance for the field of semiconductor devices, especially the field of solar cells.
Description
技术领域technical field
本发明涉及半导体叠层太阳电池材料的技术领域，特别涉及一种生长在GaAs衬底上的InGaAsN薄膜及其制备方法。The invention relates to the technical field of semiconductor stacked solar cell materials, in particular to an InGaAsN thin film grown on a GaAs substrate and a preparation method thereof.
背景技术Background technique
随着太阳能光伏发电产业和市场的迅速发展，以及在空间飞行器能源系统需求的牵引下，光伏技术不断取得重要突破：晶体硅、非晶硅、多晶硅太阳电池，III-V族化合物半导体电池，II-VI族化合物半导体电池等，越来越多的太阳电池技术日趋成熟，同时，相应的光电转换效率不断提高，使今天的光伏技术在空间和地面都得到了越来越广泛的应用。基于GaAs的III-V族化合物半导体电池技术的迅速发展是最引人瞩目、里程碑式的突破；并且GaAs基系太阳电池效率高、抗辐照性能好、耐高温、可靠性好，符合空间环境对太阳电池的要求，因此，GaAs基系太阳电池在空间科学领域正逐步取代硅系列太阳电池，成为空间太阳能发电系统的主电源。目前，基于GaAs衬底的GaAs高效多结叠层太阳电池已经获得＞41%的光电转换效率。由于GaAs材料的能带为1.42eV，而单结GaAs太阳电池只能吸收某一特定波长的太阳光，因此其光电转换效率受到限制。为了提高太阳能电池对太阳光的利用率，需要采用多结叠层太阳能电池结构，对太阳光谱进行“分割”。With the rapid development of the solar photovoltaic power generation industry and market, and driven by the demand for space vehicle energy systems, photovoltaic technology has continuously made important breakthroughs: crystalline silicon, amorphous silicon, polycrystalline silicon solar cells, III-V compound semiconductor cells, II -Group VI compound semiconductor cells, etc. More and more solar cell technologies are maturing. At the same time, the corresponding photoelectric conversion efficiency continues to increase, making today's photovoltaic technology more and more widely used in space and on the ground. The rapid development of GaAs-based III-V compound semiconductor cell technology is the most eye-catching and milestone breakthrough; and GaAs-based solar cells have high efficiency, good radiation resistance, high temperature resistance, and good reliability, which are in line with the space environment. Therefore, GaAs-based solar cells are gradually replacing silicon-based solar cells in the field of space science and become the main power source of space solar power generation systems. At present, GaAs high-efficiency multi-junction tandem solar cells based on GaAs substrates have achieved >41% photoelectric conversion efficiency. Since the energy band of the GaAs material is 1.42eV, and the single-junction GaAs solar cell can only absorb sunlight of a specific wavelength, its photoelectric conversion efficiency is limited. In order to improve the utilization rate of sunlight by solar cells, it is necessary to use a multi-junction stacked solar cell structure to "segment" the solar spectrum.
在此之上，要获得更高光电转换效率，多结叠层太阳电池的能带匹配是关键。目前常规三结GaAs系太阳电池方面，主要是GaInP/InGaAs/Ge(1.84/1.4/0.67)结构太阳电池，该体系以晶格匹配为首要考虑原则，限制了材料体系的选择，电池的转换效率提升空间非常有限。为了解决带隙失配严重制约三结叠层电池性能的问题，最新技术尝试采用GaAs为衬底的晶格匹配，且底电池带宽变为1eV的较理想能带匹配体系，这样转换效率会有所提高。除三结叠层电池外，通过理论计算，带宽为1eV的材料也可作为四结叠层太阳电池的第三结电池，这样能带匹配更为理想（1.8/1.4/1.0/0.67eV），光的转换效率会更高。而目前应用最多的带宽为1eV的材料为In0.3Ga0.7As，但是，由于In0.3Ga0.7As与GaAs晶格失配较大（晶格失配度为2.15%）会降低薄膜外延质量，晶格失配所带来的穿透位错、应力，会使外延材料体内产生大量的位错、缺陷以及表面起伏，从而恶化器件的性能，造成太阳能电池光电转换效率低。为降低缺陷密度，生长In0.3Ga0.7As需要引入生长工艺较复杂的缓冲层环节，无疑增加了不少时间和经济成本，不利于当前太阳电池发展的趋势，因此新的1eV材料有待进一步开发。研究发现，稀N半导体化合物，即在传统的III-V族半导体化合物中，并入少量的N，形成多元半导体化合物，这种材料体系具有独特的能带特性。其中，InGaAsN这种稀N半导体化合物，对于太阳电池，更是有着诱人的研究前景，因为该材料体系不仅可大范围调节带宽（理论上的带宽可达到1eV），而且当含量比为In/N=2.8时，InGaAsN晶体材料恰与GaAs衬底晶格完全匹配。这样的能隙及晶格常数特点，是太阳电池第三结最为理想的材料。但是GaInNAs薄膜的获得是十分困难的：首先，N在GaAs中的并入存在一个极限值，约为2%，而要实现InGaAsN材料带宽为1eV，则N的含量必须达到3%左右，可见要实现N在材料中的有效并入是十分困难的；其次，要使InGaAsN与GaAs晶格匹配，则材料中In/N=2.8，要精确控制这种比例难度也是很大的；最后，N的并入后，材料也十分容易发生相分离，尤其是In原子，容易在表面析出，同时相分离容易发生，In和N的均匀并入也有一定的难度。因此1eV InGaAsN的外延生长一直是研究的重点，尤其是在太阳电池领域。而根据目前外延生长技术，尤其是低温MBE技术的发展，能带为1eV的材料InGaAsN已经具备了生长的可行性。On top of this, in order to obtain higher photoelectric conversion efficiency, the energy band matching of multi-junction tandem solar cells is the key. At present, conventional triple-junction GaAs solar cells are mainly GaInP/InGaAs/Ge(1.84/1.4/0.67) solar cells. This system takes lattice matching as the primary consideration, which limits the choice of material systems and the conversion efficiency of cells. Room for improvement is very limited. In order to solve the problem that the bandgap mismatch seriously restricts the performance of triple-junction laminated cells, the latest technology tries to use GaAs as the substrate for lattice matching, and the bandwidth of the bottom cell becomes 1eV. improved. In addition to the three-junction tandem solar cell, through theoretical calculations, materials with a bandwidth of 1eV can also be used as the third junction cell of the four-junction tandem solar cell, so that the energy band matching is more ideal (1.8/1.4/1.0/0.67eV), Light conversion efficiency will be higher. At present, the most widely used material with a bandwidth of 1eV is In 0.3 Ga 0.7 As. However, due to the large lattice mismatch between In 0.3 Ga 0.7 As and GaAs (the lattice mismatch is 2.15%), the quality of thin film epitaxy will be reduced. The threading dislocations and stress caused by lattice mismatch will cause a large number of dislocations, defects and surface fluctuations in the epitaxial material, thereby deteriorating the performance of the device and resulting in low photoelectric conversion efficiency of the solar cell. In order to reduce the defect density, the growth of In 0.3 Ga 0.7 As requires the introduction of a more complex buffer layer, which undoubtedly increases a lot of time and economic costs, which is not conducive to the current development trend of solar cells. Therefore, new 1eV materials need to be further developed. Studies have found that dilute N semiconductor compounds, that is, in traditional III-V semiconductor compounds, incorporate a small amount of N to form multiple semiconductor compounds. This material system has unique energy band characteristics. Among them, InGaAsN, a dilute N semiconductor compound, has an attractive research prospect for solar cells, because this material system can not only adjust the bandwidth in a wide range (theoretical bandwidth can reach 1eV), but also when the content ratio is In/ When N=2.8, the InGaAsN crystal material is exactly matched with the GaAs substrate lattice. Such energy gap and lattice constant characteristics make it the most ideal material for the third junction of solar cells. However, it is very difficult to obtain GaInNAs thin film: firstly, there is a limit value of N incorporation in GaAs, which is about 2%, and to realize the bandwidth of InGaAsN material to be 1eV, the content of N must reach about 3%. It is very difficult to realize the effective incorporation of N in the material; secondly, to make InGaAsN and GaAs lattice match, In/N=2.8 in the material, it is also very difficult to precisely control this ratio; finally, the N After incorporation, the material is also very prone to phase separation, especially In atoms, which are easy to precipitate on the surface, and phase separation is easy to occur at the same time, and the uniform incorporation of In and N is also difficult. Therefore, the epitaxial growth of 1eV InGaAsN has been the focus of research, especially in the field of solar cells. According to the current epitaxial growth technology, especially the development of low-temperature MBE technology, the material InGaAsN with an energy band of 1eV is already feasible to grow.
发明内容Contents of the invention
为了克服现有技术的上述缺点与不足，本发明的目的在于提供一种生长在GaAs衬底上的InGaAsN薄膜，表面平整、晶体质量好。In order to overcome the above-mentioned shortcomings and deficiencies of the prior art, the object of the present invention is to provide an InGaAsN thin film grown on a GaAs substrate, which has a smooth surface and good crystal quality.
本发明的另一目的在于提供上述生长在GaAs衬底上的InGaAsN薄膜的制备方法。Another object of the present invention is to provide a method for preparing the above-mentioned InGaAsN thin film grown on a GaAs substrate.
本发明的目的通过以下技术方案实现：The object of the present invention is achieved through the following technical solutions:
一种生长在GaAs衬底上的InGaAsN薄膜，包括生长在GaAs衬底上的GaAs缓冲层、生长在GaAs缓冲层上的InGaAsN外延层薄膜。An InGaAsN thin film grown on a GaAs substrate includes a GaAs buffer layer grown on the GaAs substrate and an InGaAsN epitaxial layer thin film grown on the GaAs buffer layer.
所述GaAs缓冲层的厚度为100～150nm。The thickness of the GaAs buffer layer is 100-150 nm.
所述InGaAsN外延层薄膜的厚度为300nm～1μm。The thickness of the InGaAsN epitaxial film is 300nm-1μm.
一种生长在GaAs衬底上的InGaAsN薄膜的制备方法，包括以下步骤：A method for preparing an InGaAsN thin film grown on a GaAs substrate, comprising the following steps:
（1）清洗GaAs衬底；(1) Clean the GaAs substrate;
（2）对GaAs衬底进行除气预处理；(2) Perform degassing pretreatment on the GaAs substrate;
（3）对GaAs衬底进行脱氧化膜处理；(3) Deoxidize the GaAs substrate;
（4）生长GaAs缓冲层：GaAs衬底温度为540℃～580℃之间，Ga源温度为900℃～950℃，As源的温度为240～270℃，反应室压力3×10-5～1×10-6Torr，V-III束流比为20～30，生长速率为0.7～1.5ML/s，生长GaAs缓冲层；(4) Growth of GaAs buffer layer: GaAs substrate temperature is 540°C-580°C, Ga source temperature is 900°C-950°C, As source temperature is 240-270°C, reaction chamber pressure is 3×10 -5 ~ 1×10 -6 Torr, V-III beam current ratio of 20-30, growth rate of 0.7-1.5ML/s, growth of GaAs buffer layer;
（5）生长InGaAsN外延层薄膜：GaAs衬底温度在380～440℃，Ga源温度为900℃～950℃，As源的温度为240～270℃，反应室压力2.0～3.0×10-5Torr，在不计入N的情况下V-III束流比为20～35，产生射频N等离子体的电源功率为180～200W，N2流量为0.1～0.2sccm，生长速度1.0～1.6ML/s，生长InGaAsN外延层薄膜。(5) Growth of InGaAsN epitaxial film: GaAs substrate temperature is 380-440°C, Ga source temperature is 900-950°C, As source temperature is 240-270°C, reaction chamber pressure is 2.0-3.0×10 -5 Torr , when the V-III beam ratio is 20-35 without including N, the power supply for generating RF N plasma is 180-200W, the N2 flow rate is 0.1-0.2sccm, and the growth rate is 1.0-1.6ML/s , Growth of InGaAsN epitaxial film.
步骤（1）所述清洗GaAs衬底，具体为：Step (1) cleaning the GaAs substrate, specifically:
超声去除GaAs衬底表面粘污颗粒；经过三氯乙烯、丙酮、甲醇洗涤，去除表面有机物；将GaAs衬底放在H2SO4:H2O2:H2O溶液（3:1:1）中腐蚀1～2分钟；经HCl清洗去除表面氧化物和有机物；去离子水漂洗；清洗后的GaAs衬底用经过过滤的干燥氮气吹干。Ultrasonic removal of dirt particles on the surface of the GaAs substrate; washing with trichlorethylene, acetone, and methanol to remove surface organic matter; placing the GaAs substrate in H 2 SO 4 :H 2 O 2 :H 2 O solution (3:1:1 ) for 1 to 2 minutes; wash with HCl to remove surface oxides and organic matter; rinse with deionized water; clean the GaAs substrate with filtered dry nitrogen.
步骤（2）所述对GaAs衬底进行除气预处理，具体为：In step (2), the degassing pretreatment of the GaAs substrate is carried out, specifically:
将清洗完毕后的GaAs衬底送入分子束外延进样室预除气半小时；再送入传递室300～400℃除气1～1.5小时，完成除气后送入生长室。The cleaned GaAs substrate is sent to the molecular beam epitaxy sampling chamber for pre-degassing for half an hour; then sent to the transfer chamber for degassing at 300-400°C for 1-1.5 hours, and then sent to the growth chamber after degassing is completed.
步骤（3）所述对GaAs衬底进行脱氧化膜处理，具体为：In step (3), the GaAs substrate is subjected to deoxidation film treatment, specifically:
在砷束流保护下，将GaAs衬底温度升至600～650℃，高温烘烤10～15分钟。Under the protection of the arsenic beam, the temperature of the GaAs substrate is raised to 600-650° C., and baked at a high temperature for 10-15 minutes.
所述GaAs缓冲层的厚度为100～150nm。The thickness of the GaAs buffer layer is 100-150 nm.
所述InGaAsN外延层薄膜的厚度为300nm～1μm。The thickness of the InGaAsN epitaxial film is 300nm-1μm.
与现有技术相比，本发明具有以下优点和有益效果：Compared with the prior art, the present invention has the following advantages and beneficial effects:
（1）本发明的生长在GaAs衬底上的InGaAsN薄膜，先在GaAs衬底上生长GaAs缓冲层，结构简单，得到的InGaAsN薄膜表面平整、成分均匀，有利于实际的生产应用。(1) In the InGaAsN film grown on the GaAs substrate of the present invention, a GaAs buffer layer is first grown on the GaAs substrate, the structure is simple, and the obtained InGaAsN film has a smooth surface and uniform composition, which is beneficial to actual production and application.
（2）本发明的制备方法，应用低温MBE技术，得到的生长在GaAs衬底上的InGaAsN薄膜，带宽为1eV，在技术领域上是一个新的突破，能对半导体器件领域，尤其是太阳电池领域，有着积极的促进意义。(2) The preparation method of the present invention uses low-temperature MBE technology to obtain an InGaAsN thin film grown on a GaAs substrate with a bandwidth of 1eV, which is a new breakthrough in the technical field and can be used in the field of semiconductor devices, especially solar cells. field, has a positive promotion significance.
（3）本发明的制备方法得到的生长在GaAs衬底上的InGaAsN薄膜，实现了四种组分均匀并入，有效解决了生长InGaAsN容易出现相分离的现象，从而得到较高质量的四元薄膜材料。(3) The InGaAsN film grown on the GaAs substrate obtained by the preparation method of the present invention realizes the uniform incorporation of four components, effectively solving the phenomenon that the growth of InGaAsN is prone to phase separation, thereby obtaining a higher quality quaternary film material.
附图说明Description of drawings
图1为本发明的实施例制备的生长在GaAs衬底上的InGaAsN薄膜的示意图。FIG. 1 is a schematic diagram of an InGaAsN thin film grown on a GaAs substrate prepared in an embodiment of the present invention.
图2为本发明的实施例制备的生长在GaAs衬底上的InGaAsN薄膜的室温荧光光谱图。Fig. 2 is a room temperature fluorescence spectrum diagram of an InGaAsN thin film grown on a GaAs substrate prepared in an embodiment of the present invention.
图3为本发明的实施例制备的生长在GaAs衬底上的InGaAsN薄膜的扫描电子显微镜图。Fig. 3 is a scanning electron microscope image of an InGaAsN thin film grown on a GaAs substrate prepared in an embodiment of the present invention.
图4为本发明的实施例制备的生长在GaAs衬底上的InGaAsN薄膜二次离子质谱图。FIG. 4 is a secondary ion mass spectrum of an InGaAsN thin film grown on a GaAs substrate prepared in an embodiment of the present invention.
具体实施方式Detailed ways
下面结合实施例，对本发明作进一步地详细说明，但本发明的实施方式不限于此。The present invention will be described in further detail below in conjunction with the examples, but the embodiments of the present invention are not limited thereto.
实施例1Example 1
本实施例的生长在GaAs衬底上的InGaAsN薄膜的制备方法，包括以下步骤：The preparation method of the InGaAsN thin film grown on the GaAs substrate of the present embodiment comprises the following steps:
（1）清洗GaAs衬底，具体为：(1) Clean the GaAs substrate, specifically:
采用（001）晶向的n-GaAs衬底；超声去除GaAs衬底表面粘污颗粒；经过三氯乙烯、丙酮、甲醇洗涤，去除表面有机物；将GaAs衬底放在H2SO4:H2O2:H2O溶液（3:1:1）中腐蚀1分钟；经HCl清洗去除表面氧化物和有机物；去离子水漂洗；清洗后的GaAs衬底用经过过滤的干燥氮气吹干。Use n-GaAs substrate with (001) crystal orientation; ultrasonically remove the dirt particles on the surface of the GaAs substrate; wash with trichlorethylene, acetone, and methanol to remove surface organic matter; place the GaAs substrate in H 2 SO 4 :H 2 Etch in O 2 :H 2 O solution (3:1:1) for 1 minute; wash with HCl to remove surface oxides and organic matter; rinse with deionized water; clean the GaAs substrate with filtered dry nitrogen.
（2）对GaAs衬底进行除气预处理，具体为：(2) Perform degassing pretreatment on the GaAs substrate, specifically:
将清洗完毕后的GaAs衬底送入分子束外延进样室预除气半小时；再送入传递室300℃除气1.5小时，完成除气后送入生长室；Send the cleaned GaAs substrate into the molecular beam epitaxy sampling chamber for pre-degassing for half an hour; then send it into the transfer chamber for degassing at 300°C for 1.5 hours, and then send it to the growth chamber after degassing;
（3）对GaAs衬底进行脱氧化膜处理，具体为：在砷束流保护下，将GaAs衬底温度升至600℃，高温烘烤15分钟。(3) Perform deoxidation film treatment on the GaAs substrate, specifically: under the protection of the arsenic beam, raise the temperature of the GaAs substrate to 600° C., and bake at high temperature for 15 minutes.
（4）生长GaAs缓冲层：GaAs衬底温度为540℃，Ga源温度为900℃，As源的温度为240℃，反应室压力1×10-6Torr，V-III束流比为20，生长速率为0.7ML/s，生长厚度为100nm的GaAs缓冲层；本步骤对InGaAsN外延层薄膜表面的平整度起着重要作用。(4) Growth of GaAs buffer layer: GaAs substrate temperature is 540°C, Ga source temperature is 900°C, As source temperature is 240°C, reaction chamber pressure is 1×10 -6 Torr, V-III beam ratio is 20, The growth rate is 0.7ML/s, and a GaAs buffer layer with a thickness of 100nm is grown; this step plays an important role in the smoothness of the surface of the InGaAsN epitaxial film.
（5）生长InGaAsN外延层薄膜：GaAs衬底温度为380℃，Ga源温度为900℃，As源的温度为240℃，反应室压力为3.0×10-5Torr，在不计入N的情况下V-III束流比为20，产生射频N等离子体的电源功率为180W，N2流量为0.1sccm、生长速度1.0ML/s，生长厚度为300nm的InGaAsN外延层薄膜。(5) Growth of InGaAsN epitaxial film: GaAs substrate temperature is 380°C, Ga source temperature is 900°C, As source temperature is 240°C, reaction chamber pressure is 3.0×10 -5 Torr, when N is not included The V-III beam ratio is 20, the power supply for generating radio frequency N plasma is 180W, the N 2 flow rate is 0.1sccm, the growth rate is 1.0ML/s, and the InGaAsN epitaxial film with a thickness of 300nm is grown.
如图1所示，本实施例制备的生长在GaAs衬底上的InGaAsN薄膜，包括生长在GaAs衬底11上的GaAs缓冲层12、生长在GaAs缓冲层12上的InGaAsN外延层薄膜13。As shown in FIG. 1 , the InGaAsN film grown on a GaAs substrate prepared in this embodiment includes a GaAs buffer layer 12 grown on a GaAs substrate 11 and an InGaAsN epitaxial film 13 grown on the GaAs buffer layer 12 .
图2为本实施例制备的生长在GaAs衬底上的InGaAsN薄膜的室温荧光光谱图，由图2可知，InGaAsN外延层薄膜的带宽为1eV，说明本发明的制备方法能成功生长InGaAsN。Fig. 2 is the room temperature fluorescence spectrum of the InGaAsN thin film grown on the GaAs substrate prepared in this embodiment. It can be seen from Fig. 2 that the bandwidth of the InGaAsN epitaxial layer thin film is 1eV, indicating that the preparation method of the present invention can successfully grow InGaAsN.
图3为本实施例制备的生长在GaAs衬底上的InGaAsN薄膜的扫描电子显微镜图。由图3可知，InGaAsN外延层薄膜的表面较平整，不存在In原子的偏析现象，说明本发明制备方法能有效避免InGaAsN相分离，提高薄膜的质量。FIG. 3 is a scanning electron microscope image of the InGaAsN thin film grown on the GaAs substrate prepared in this embodiment. It can be seen from FIG. 3 that the surface of the InGaAsN epitaxial film is relatively smooth, and there is no segregation phenomenon of In atoms, which shows that the preparation method of the present invention can effectively avoid InGaAsN phase separation and improve the quality of the film.
图4为本实施例制备的生长在GaAs衬底上的InGaAsN薄膜二次离子质谱图。由图4可知，InGaAsN外延层薄膜各元素在材料中的分布情况。随着二次离子刻蚀时间的增大，四种元素的强度信息均比较稳定，说明各元素在薄膜的纵向深度上是均匀分布的，尤其对于In和N原子，这种均匀分布是十分难得的。FIG. 4 is a secondary ion mass spectrum of the InGaAsN thin film grown on the GaAs substrate prepared in this embodiment. It can be known from Figure 4, the distribution of each element in the InGaAsN epitaxial film in the material. As the secondary ion etching time increases, the intensity information of the four elements is relatively stable, indicating that the elements are uniformly distributed in the longitudinal depth of the film, especially for In and N atoms, such a uniform distribution is very rare of.
本发明的GaAs缓冲层和InGaAsN外延层薄膜均采用分子束外延生长方法，不仅可对N原子实行有效并入，从而获得带宽为1eV的四元半导体材料体系又能提高薄膜表面的平整度，避免In原子的表面偏析现象。Both the GaAs buffer layer and the InGaAsN epitaxial layer film of the present invention adopt the molecular beam epitaxy growth method, which not only can effectively incorporate N atoms, thereby obtaining a quaternary semiconductor material system with a bandwidth of 1eV, but also improving the flatness of the film surface to avoid Surface segregation of In atoms.
实施例2Example 2
本实施例的生长在GaAs衬底上的InGaAsN薄膜的制备方法，包括以下步骤：The preparation method of the InGaAsN thin film grown on the GaAs substrate of the present embodiment comprises the following steps:
（1）清洗GaAs衬底，具体为：(1) Clean the GaAs substrate, specifically:
采用（001）晶向的n-GaAs衬底；超声去除GaAs衬底表面粘污颗粒；经过三氯乙烯、丙酮、甲醇洗涤，去除表面有机物；将GaAs衬底放在H2SO4:H2O2:H2O溶液（3:1:1）中腐蚀2分钟；经HCl清洗去除表面氧化物和有机物；去离子水漂洗；清洗后的GaAs衬底用经过过滤的干燥氮气吹干。Use n-GaAs substrate with (001) crystal orientation; ultrasonically remove the dirt particles on the surface of the GaAs substrate; wash with trichlorethylene, acetone, and methanol to remove surface organic matter; place the GaAs substrate in H 2 SO 4 :H 2 Etching in O 2 :H 2 O solution (3:1:1) for 2 minutes; cleaning with HCl to remove surface oxides and organic matter; rinsing with deionized water; and drying the cleaned GaAs substrate with filtered dry nitrogen.
（2）对GaAs衬底进行除气预处理，具体为：(2) Perform degassing pretreatment on the GaAs substrate, specifically:
将清洗完毕后的GaAs衬底送入分子束外延进样室预除气半小时；再送入传递室400℃除气1小时，完成除气后送入生长室；Send the cleaned GaAs substrate into the molecular beam epitaxy sampling chamber for pre-degassing for half an hour; then send it into the transfer chamber for degassing at 400°C for 1 hour, and then send it to the growth chamber after degassing;
（3）对GaAs衬底进行脱氧化膜处理，具体为：在砷束流保护下，将GaAs衬底温度升至650℃，高温烘烤10分钟。(3) Perform deoxidation film treatment on the GaAs substrate, specifically: under the protection of the arsenic beam, raise the temperature of the GaAs substrate to 650° C., and bake at high temperature for 10 minutes.
（4）生长GaAs缓冲层：GaAs衬底温度为580℃，Ga源温度为950℃，As源的温度为270℃，反应室压力为3×10-5Torr，V-III束流比为30，生长速率为1.5ML/s，生长厚度为150nm的GaAs缓冲层；本步骤对InGaAsN外延层薄膜表面的平整度起着重要作用。(4) Growth of GaAs buffer layer: GaAs substrate temperature is 580°C, Ga source temperature is 950°C, As source temperature is 270°C, reaction chamber pressure is 3×10 -5 T o rr, V-III beam current ratio 30, the growth rate is 1.5ML/s, and a GaAs buffer layer with a thickness of 150nm is grown; this step plays an important role in the flatness of the InGaAsN epitaxial film surface.
（5）生长InGaAsN外延层薄膜：GaAs衬底温度在440℃，Ga源温度为950℃，As源的温度为270℃，反应室压力2.0×10-5Torr，在不计入N的情况下V-III束流比为35，产生射频N等离子体的电源功率为200W，N2流量为0.2sccm，生长速度1.6ML/s，生长厚度为1.0μm的InGaAsN外延层薄膜。(5) Growth of InGaAsN epitaxial film: GaAs substrate temperature is 440°C, Ga source temperature is 950°C, As source temperature is 270°C, reaction chamber pressure is 2.0×10 -5 Torr, without including N The V-III beam ratio is 35, the power supply for generating RF N plasma is 200W, the N 2 flow rate is 0.2sccm, the growth rate is 1.6ML/s, and the InGaAsN epitaxial film with a thickness of 1.0μm is grown.
本实施例制备的生长在GaAs衬底上的InGaAsN薄膜，包括生长在GaAs衬底上的GaAs缓冲层、生长在GaAs缓冲层上的InGaAsN外延层薄膜。The InGaAsN thin film grown on the GaAs substrate prepared in this embodiment includes a GaAs buffer layer grown on the GaAs substrate and an InGaAsN epitaxial thin film grown on the GaAs buffer layer.
本实施例制备得到的生长在GaAs衬底上的InGaAsN薄膜测试结果与实施例1类似，在此不再赘述。The test results of the InGaAsN thin film grown on the GaAs substrate prepared in this embodiment are similar to those in Embodiment 1, and will not be repeated here.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受所述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the embodiment, and any other changes, modifications, substitutions and combinations made without departing from the spirit and principle of the present invention , simplification, all should be equivalent replacement methods, and are all included in the protection scope of the present invention.
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