CN113481593B - Preparation method of light-emitting diode epitaxial wafer with AlN - Google Patents
Preparation method of light-emitting diode epitaxial wafer with AlN Download PDFInfo
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Abstract
本公开提供了一种具有AlN的发光二极管外延片的制备方法,属于发光二极管技术领域。交替在衬底的表面溅射第一AlN膜与第二AlN膜以最终形成AlN缓冲层。并且溅射第一AlN膜时的靶间距为第一靶间距,溅射第二AlN膜时的靶间距为第二靶间距,第一靶间距大于第二靶间距。较大的第一靶间距溅射得到的第一AlN膜的厚度与均匀性会较好。较小的第二靶间距溅射第二AlN膜的速度会较快,提高第二AlN膜的沉积速率。而交替得到的第一AlN膜与第二AlN膜的内部应力得到释放,AlN缓冲层的整体质量得到提高,并且AlN缓冲层的生长速率也得到提高。降低发光二极管外延片的制备周期的同时有效提高发光二极管外延片的晶体质量。
The disclosure provides a method for preparing a light-emitting diode epitaxial wafer with AlN, which belongs to the technical field of light-emitting diodes. The first AlN film and the second AlN film are alternately sputtered on the surface of the substrate to finally form an AlN buffer layer. And the target distance when sputtering the first AlN film is the first target distance, the target distance when sputtering the second AlN film is the second target distance, and the first target distance is larger than the second target distance. The thickness and uniformity of the first AlN film obtained by sputtering with a larger first target distance will be better. The smaller the second target distance, the sputtering speed of the second AlN film will be faster, and the deposition rate of the second AlN film will be improved. The internal stress of the alternately obtained first AlN film and the second AlN film is released, the overall quality of the AlN buffer layer is improved, and the growth rate of the AlN buffer layer is also increased. The crystal quality of the epitaxial wafer of the light emitting diode is effectively improved while reducing the preparation period of the epitaxial wafer of the light emitting diode.
Description
技术领域technical field
本公开涉及到了发光二极管技术领域,特别涉及到一种具有AlN的发光二极管外延片的制备方法。The present disclosure relates to the technical field of light emitting diodes, in particular to a method for preparing a light emitting diode epitaxial wafer with AlN.
背景技术Background technique
发光二极管是一种应用非常广泛的发光器件,常用于通信号灯、汽车内外灯、城市照明和景观照明等,发光二极管外延片则是用于制备发光二极管的基础结构。发光二极管外延片通常包括衬底及衬底上依次层叠的AlN缓冲层、n型GaN层、多量子阱层及p型GaN层。Light-emitting diodes are widely used light-emitting devices, often used in traffic lights, car interior and exterior lights, urban lighting and landscape lighting, etc., and light-emitting diode epitaxial wafers are the basic structure used to prepare light-emitting diodes. A light-emitting diode epitaxial wafer usually includes a substrate and an AlN buffer layer, an n-type GaN layer, a multi-quantum well layer and a p-type GaN layer stacked sequentially on the substrate.
AlN缓冲层可以缓解n型GaN层与衬底之间的晶格失配。为提高AlN缓冲层的晶体质量,但AlN缓冲层的生长周期一般比较长,且最终得到的AlN缓冲层的质量也不够好。The AlN buffer layer can alleviate the lattice mismatch between the n-type GaN layer and the substrate. In order to improve the crystal quality of the AlN buffer layer, the growth period of the AlN buffer layer is generally relatively long, and the quality of the finally obtained AlN buffer layer is not good enough.
发明内容Contents of the invention
本公开实施例提供了一种具有AlN的发光二极管外延片的制备方法,可以降低发光二极管外延片的制备周期的同时有效提高发光二极管外延片的晶体质量。所述技术方案如下:The embodiment of the present disclosure provides a method for preparing a light-emitting diode epitaxial wafer with AlN, which can reduce the production cycle of the light-emitting diode epitaxial wafer and effectively improve the crystal quality of the light-emitting diode epitaxial wafer. Described technical scheme is as follows:
本公开实施例提供了一种具有AlN的发光二极管外延片的制备方法,所述具有AlN的发光二极管外延片的制备方法包括:An embodiment of the present disclosure provides a method for preparing a light-emitting diode epitaxial wafer with AlN, and the method for preparing the light-emitting diode epitaxial wafer with AlN includes:
提供一位于磁控溅射装置中的衬底,所述磁控溅射装置中的靶材的表面与所述衬底的表面正对且相互平行,所述靶材的表面与所述衬底的表面之间的垂直距离为靶间距;Provide a substrate located in the magnetron sputtering device, the surface of the target in the magnetron sputtering device is directly opposite to the surface of the substrate and parallel to each other, the surface of the target and the substrate The vertical distance between the surfaces of is the target spacing;
交替在所述衬底的表面溅射第一AlN膜与第二AlN膜以最终形成AlN缓冲层,溅射所述第一AlN膜时所述靶间距为第一靶间距,溅射所述第二AlN膜时所述靶间距为第二靶间距,所述第一靶间距大于所述第二靶间距;Alternately sputtering the first AlN film and the second AlN film on the surface of the substrate to finally form an AlN buffer layer, when sputtering the first AlN film, the target distance is the first target distance, and sputtering the first AlN film When two AlN films are used, the target distance is the second target distance, and the first target distance is greater than the second target distance;
在所述AlN缓冲层上依次生长n型GaN层、多量子阱层与p型GaN层。An n-type GaN layer, a multi-quantum well layer and a p-type GaN layer are grown sequentially on the AlN buffer layer.
可选地,所述第一靶间距为70mm~100mm,所述第二靶间距为40mm~70mm。Optionally, the first target distance is 70 mm to 100 mm, and the second target distance is 40 mm to 70 mm.
可选地,所述第一靶间距与所述第二靶间距之差的绝对值为20mm~50mm。Optionally, the absolute value of the difference between the first target distance and the second target distance is 20 mm to 50 mm.
可选地,所述第一AlN膜的厚度为0.1~5nm。Optionally, the thickness of the first AlN film is 0.1-5 nm.
可选地,所述第二AlN膜的厚度为2~20nm。Optionally, the thickness of the second AlN film is 2-20 nm.
可选地,所述第二AlN膜的厚度与所述第一AlN膜的厚度之比为5~20。Optionally, a ratio of the thickness of the second AlN film to the thickness of the first AlN film is 5-20.
可选地,所述制备方法还包括:Optionally, the preparation method also includes:
溅射所述第一AlN膜之后,间隔20~100s,进行所述第二AlN膜的溅射。After the first AlN film is sputtered, the second AlN film is sputtered at an interval of 20-100 s.
可选地,所述第一AlN膜的溅射温度为500℃~800℃,所述第一AlN膜的溅射压力为4~10mtorr。Optionally, the sputtering temperature of the first AlN film is 500°C-800°C, and the sputtering pressure of the first AlN film is 4-10mtorr.
可选地,在所述衬底上生长AlN缓冲层之后,在所述AlN缓冲层上生长n型GaN层之前,Optionally, after growing the AlN buffer layer on the substrate, before growing an n-type GaN layer on the AlN buffer layer,
对所述AlN缓冲层进行10~15min的热处理。Perform heat treatment on the AlN buffer layer for 10-15 minutes.
可选地,对所述AlN缓冲层进行热处理的温度为1100~1200℃。Optionally, the temperature for heat treatment of the AlN buffer layer is 1100-1200°C.
本公开实施例提供的技术方案带来的有益效果包括:The beneficial effects brought by the technical solutions provided by the embodiments of the present disclosure include:
将衬底放在磁控溅射装置中,并使磁控溅射装置中的靶材的表面与衬底的表面正对且相互平行,靶材的表面与衬底的表面之间的垂直距离为靶间距。需要在衬底上溅射AlN缓冲层时,可以交替在衬底的表面溅射第一AlN膜与第二AlN膜以最终形成AlN缓冲层。并且溅射第一AlN膜时的靶间距为第一靶间距,溅射第二AlN膜时的靶间距为第二靶间距,第一靶间距大于第二靶间距。较大的第一靶间距溅射得到的第一AlN膜的厚度与均匀性会较好,且可以保证在第一AlN膜上生长的第二AlN膜的质量较好。较小的第二靶间距溅射第二AlN膜的速度会较快,可以提高第二AlN膜的沉积速率,且由于第二靶间距的减小导致的第二AlN膜均匀性的降低可以被第一AlN膜的质量的提高抵消,整体的质量仍可以保证。而交替得到的第一AlN膜与第二AlN膜的内部应力可以得到释放,最终得到的AlN缓冲层的内部由应力导致的内部缺陷较少,AlN缓冲层的整体质量可以得到提高,并且AlN缓冲层的生长速率也可以得到提高。降低发光二极管外延片的制备周期的同时有效提高发光二极管外延片的晶体质量。Put the substrate in the magnetron sputtering device, and make the surface of the target in the magnetron sputtering device face the surface of the substrate and be parallel to each other, the vertical distance between the surface of the target and the surface of the substrate is the target distance. When the AlN buffer layer needs to be sputtered on the substrate, the first AlN film and the second AlN film can be alternately sputtered on the surface of the substrate to finally form the AlN buffer layer. And the target distance when sputtering the first AlN film is the first target distance, the target distance when sputtering the second AlN film is the second target distance, and the first target distance is larger than the second target distance. The thickness and uniformity of the first AlN film obtained by sputtering with a larger first target distance will be better, and it can ensure that the quality of the second AlN film grown on the first AlN film is better. The speed of sputtering the second AlN film with the smaller second target spacing will be faster, which can improve the deposition rate of the second AlN film, and the reduction of the uniformity of the second AlN film due to the reduction of the second target spacing can be eliminated. The improvement of the quality of the first AlN film is offset, and the overall quality can still be guaranteed. The internal stress of the alternately obtained first AlN film and the second AlN film can be released, and the internal defects of the finally obtained AlN buffer layer caused by stress are less, the overall quality of the AlN buffer layer can be improved, and the AlN buffer layer The growth rate of the layers can also be increased. The crystal quality of the epitaxial wafer of the light emitting diode is effectively improved while reducing the preparation cycle of the epitaxial wafer of the light emitting diode.
附图说明Description of drawings
为了更清楚地说明本公开实施例中的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本公开的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure, the drawings that need to be used in the description of the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present disclosure. For those skilled in the art, other drawings can also be obtained based on these drawings without creative effort.
图1是本公开实施例提供的一种具有AlN的发光二极管外延片的制备方法流程图;FIG. 1 is a flow chart of a method for preparing a light-emitting diode epitaxial wafer with AlN provided by an embodiment of the present disclosure;
图2是本公开实施例提供的磁控溅射装置的内部结构简化图;Fig. 2 is a simplified diagram of the internal structure of a magnetron sputtering device provided by an embodiment of the present disclosure;
图3是本公开实施例提供的一种发光二极管外延片的结构示意图;FIG. 3 is a schematic structural view of a light emitting diode epitaxial wafer provided by an embodiment of the present disclosure;
图4是本公开实施例提供的另一种具有AlN的发光二极管外延片的制备方法流程图;4 is a flow chart of another method for preparing a light-emitting diode epitaxial wafer with AlN provided by an embodiment of the present disclosure;
图5是本公开实施例提供的另一种发光二极管外延片的结构示意图。FIG. 5 is a schematic structural diagram of another light-emitting diode epitaxial wafer provided by an embodiment of the present disclosure.
具体实施方式detailed description
为使本公开的目的、技术方案和优点更加清楚,下面将结合附图对本公开实施方式作进一步地详细描述。In order to make the purpose, technical solution and advantages of the present disclosure clearer, the implementation manners of the present disclosure will be further described in detail below in conjunction with the accompanying drawings.
除非另作定义,此处使用的技术术语或者科学术语应当为本公开所属领域内具有一般技能的人士所理解的通常意义。本公开专利申请说明书以及权利要求书中使用的“第一”、“第二”、“第三”以及类似的词语并不表示任何顺序、数量或者重要性,而只是用来区分不同的组成部分。同样,“一个”或者“一”等类似词语也不表示数量限制,而是表示存在至少一个。“包括”或者“包含”等类似的词语意指出现在“包括”或者“包含”前面的元件或者物件涵盖出现在“包括”或者“包含”后面列举的元件或者物件及其等同,并不排除其他元件或者物件。“连接”或者“相连”等类似的词语并非限定于物理的或者机械的连接,而是可以包括电性的连接,不管是直接的还是间接的。“上”、“下”、“左”、“右”、“顶”、“底”等仅用于表示相对位置关系,当被描述对象的绝对位置改变后,则所述相对位置关系也可能相应地改变。Unless otherwise defined, the technical terms or scientific terms used herein shall have the usual meanings understood by those having ordinary skill in the art to which the present disclosure belongs. "First", "second", "third" and similar words used in the specification and claims of this disclosure do not indicate any order, quantity or importance, but are only used to distinguish different components . Likewise, words like "a" or "one" do not denote a limitation in quantity, but indicate that there is at least one. Words such as "comprises" or "comprising" and similar terms mean that the elements or items listed before "comprising" or "comprising" include the elements or items listed after "comprising" or "comprising" and their equivalents, and do not exclude other component or object. Words such as "connected" or "connected" are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "Down", "Left", "Right", "Top", "Bottom" and so on are only used to indicate the relative positional relationship. When the absolute position of the described object changes, the relative positional relationship may also be Change accordingly.
图1是本公开实施例提供的一种具有AlN的发光二极管外延片的制备方法流程图,如图1所示,该具有AlN的发光二极管外延片的制备方法包括:Fig. 1 is a flow chart of a method for preparing a light-emitting diode epitaxial wafer with AlN provided by an embodiment of the present disclosure. As shown in Fig. 1, the preparation method of the light-emitting diode epitaxial wafer with AlN includes:
S101:提供一位于磁控溅射装置中的衬底,磁控溅射装置中的靶材的表面与衬底的表面正对且相互平行,靶材的表面与衬底的表面之间的垂直距离为靶间距。S101: Provide a substrate located in a magnetron sputtering device, the surface of the target in the magnetron sputtering device is directly opposite to and parallel to the surface of the substrate, and the vertical distance between the surface of the target and the surface of the substrate is The distance is the target pitch.
S102:交替在衬底的表面溅射第一AlN膜与第二AlN膜以最终形成AlN缓冲层,溅射第一AlN膜时的靶间距为第一靶间距,溅射第二AlN膜时的靶间距为第二靶间距,第一靶间距大于第二靶间距。S102: Alternately sputtering the first AlN film and the second AlN film on the surface of the substrate to finally form an AlN buffer layer, the target pitch when sputtering the first AlN film is the first target pitch, and the target pitch when sputtering the second AlN film The target pitch is the second target pitch, and the first target pitch is greater than the second target pitch.
S103:在AlN缓冲层上依次生长n型GaN层、多量子阱层与p型GaN层。S103: growing an n-type GaN layer, a multi-quantum well layer, and a p-type GaN layer sequentially on the AlN buffer layer.
将衬底放在磁控溅射装置中,并使磁控溅射装置中的靶材的表面与衬底的表面正对且相互平行,靶材的表面与衬底的表面之间的垂直距离为靶间距。需要在衬底上溅射AlN缓冲层时,可以交替在衬底的表面溅射第一AlN膜与第二AlN膜以最终形成AlN缓冲层。并且溅射第一AlN膜时的靶间距为第一靶间距,溅射第二AlN膜时的靶间距为第二靶间距,第一靶间距大于第二靶间距。较大的第一靶间距溅射得到的第一AlN膜的厚度与均匀性会较好,且可以保证在第一AlN膜上生长的第二AlN膜的质量较好。较小的第二靶间距溅射第二AlN膜的速度会较快,可以提高第二AlN膜的沉积速率,且由于第二靶间距的减小导致的第二AlN膜均匀性的降低可以被第一AlN膜的质量的提高抵消,整体的质量仍可以保证。而交替得到的第一AlN膜与第二AlN膜的内部应力可以得到释放,最终得到的AlN缓冲层的内部由应力导致的内部缺陷较少,AlN缓冲层的整体质量可以得到提高,并且AlN缓冲层的生长速率也可以得到提高。降低发光二极管外延片的制备周期的同时有效提高发光二极管外延片的晶体质量。Put the substrate in the magnetron sputtering device, and make the surface of the target in the magnetron sputtering device face the surface of the substrate and be parallel to each other, the vertical distance between the surface of the target and the surface of the substrate is the target distance. When the AlN buffer layer needs to be sputtered on the substrate, the first AlN film and the second AlN film can be alternately sputtered on the surface of the substrate to finally form the AlN buffer layer. And the target distance when sputtering the first AlN film is the first target distance, the target distance when sputtering the second AlN film is the second target distance, and the first target distance is larger than the second target distance. The thickness and uniformity of the first AlN film obtained by sputtering with a larger first target distance will be better, and it can ensure that the quality of the second AlN film grown on the first AlN film is better. The speed of sputtering the second AlN film with the smaller second target spacing will be faster, which can improve the deposition rate of the second AlN film, and the reduction of the uniformity of the second AlN film due to the reduction of the second target spacing can be eliminated. The improvement of the quality of the first AlN film is offset, and the overall quality can still be guaranteed. The internal stress of the alternately obtained first AlN film and the second AlN film can be released, and the internal defects of the finally obtained AlN buffer layer caused by stress are less, the overall quality of the AlN buffer layer can be improved, and the AlN buffer layer The growth rate of the layers can also be increased. The crystal quality of the epitaxial wafer of the light emitting diode is effectively improved while reducing the preparation cycle of the epitaxial wafer of the light emitting diode.
为便于理解,此处可提供图2,图2是本公开实施例提供的磁控溅射装置的内部结构简化图,参考图2可知,衬底1与靶材100均位于磁控溅射装置的腔内,衬底1固定于磁控溅射装置的腔的顶部,靶材100固定于磁控溅射装置的腔的底部,靶材100的表面为一平面,且靶材100的表面与衬底1的表面相对且相互平行,靶间距在图2中的标识为C。For ease of understanding, FIG. 2 can be provided here. FIG. 2 is a simplified diagram of the internal structure of the magnetron sputtering device provided by the embodiment of the present disclosure. Referring to FIG. 2, it can be known that the
图3是本公开实施例提供的一种发光二极管外延片的结构示意图,参考图3可知,本公开实施例提供了一种发光二极管外延片,发光二极管外延片包括衬底1及依次层叠在衬底1上的AlN缓冲层2、n型GaN层3、多量子阱层4及p型GaN层5。FIG. 3 is a schematic structural view of a light emitting diode epitaxial wafer provided by an embodiment of the present disclosure. Referring to FIG. 3, it can be known that an embodiment of the present disclosure provides a light emitting diode epitaxial wafer.
需要说明的是,图3中所提供的发光二极管外延片的结构仅用于示意,图1中所示的具有AlN的发光二极管外延片的制备方法也可应用于其他具有更多层次的发光二极管外延片,本公开对此不做限制。It should be noted that the structure of the light-emitting diode epitaxial wafer provided in Figure 3 is only for illustration, and the preparation method of the light-emitting diode epitaxial wafer with AlN shown in Figure 1 can also be applied to other light-emitting diodes with more layers Epitaxial wafer, the present disclosure does not limit it.
图4是本公开实施例提供的另一种具有AlN的发光二极管外延片的制备方法流程图,如图4所示,该具有AlN的发光二极管外延片的制备方法包括:FIG. 4 is a flow chart of another method for preparing a light emitting diode epitaxial wafer with AlN provided by an embodiment of the present disclosure. As shown in FIG. 4 , the preparation method of the light emitting diode epitaxial wafer with AlN includes:
S201:提供一衬底。S201: Provide a substrate.
其中,衬底可为蓝宝石衬底。易于实现与制作。Wherein, the substrate may be a sapphire substrate. Easy to implement and make.
S202:将衬底放入磁控溅射装置中,磁控溅射装置中的靶材的表面与衬底的表面正对且相互平行,靶材的表面与衬底的表面之间的垂直距离为靶间距。S202: Put the substrate into the magnetron sputtering device, the surface of the target in the magnetron sputtering device is facing the surface of the substrate and parallel to each other, the vertical distance between the surface of the target and the surface of the substrate is the target distance.
可选地,步骤S202还可包括:在氢气气氛下,处理衬底用于生长外延层的表面5~6min。Optionally, step S202 may further include: treating the surface of the substrate for growing the epitaxial layer for 5-6 minutes in a hydrogen atmosphere.
示例性地,处理衬底用于生长外延层的表面时,反应腔的温度可为1000~1100℃,反应腔的压力可为200~500torr。能够有效清除衬底上所存在的杂质,保证最终得到的衬底上的外延结构的质量较好。Exemplarily, when the substrate is processed to grow the surface of the epitaxial layer, the temperature of the reaction chamber may be 1000-1100° C., and the pressure of the reaction chamber may be 200-500 torr. Impurities existing on the substrate can be effectively removed to ensure better quality of the finally obtained epitaxial structure on the substrate.
S203:交替在衬底的表面溅射第一AlN膜与第二AlN膜以最终形成AlN缓冲层,溅射第一AlN膜时的靶间距为第一靶间距,溅射第二AlN膜时的靶间距为第二靶间距,第一靶间距大于第二靶间距。S203: Alternately sputtering the first AlN film and the second AlN film on the surface of the substrate to finally form an AlN buffer layer, the target pitch when sputtering the first AlN film is the first target pitch, and the target pitch when sputtering the second AlN film The target pitch is the second target pitch, and the first target pitch is greater than the second target pitch.
可选地,AlN缓冲层的生长厚度可为10~50nm。Optionally, the growth thickness of the AlN buffer layer may be 10-50 nm.
AlN缓冲层的生长厚度在以上范围内,可以有效提高最终得到的AlN缓冲层的晶体质量,保证在AlN缓冲层上生长的外延材料的质量。The growth thickness of the AlN buffer layer within the above range can effectively improve the crystal quality of the finally obtained AlN buffer layer and ensure the quality of the epitaxial material grown on the AlN buffer layer.
可选地,第一AlN膜的溅射温度为500℃~800℃,第一AlN膜的溅射压力为4~10mtorr。Optionally, the sputtering temperature of the first AlN film is 500° C.˜800° C., and the sputtering pressure of the first AlN film is 4˜10 mtorr.
第一AlN膜的溅射温度与溅射压力在以上范围内时,可以得到质量良好的第一AlN膜。When the sputtering temperature and sputtering pressure of the first AlN film are within the above range, the first AlN film with good quality can be obtained.
示例性地,第二AlN膜的溅射温度与第一AlN膜的溅射温度相同,第二AlN膜的溅射压力与第一AlN膜的溅射压力相同。可以保证最终得到的AlN缓冲层的质量较好的同时有效提高AlN缓冲层的成形效率。Exemplarily, the sputtering temperature of the second AlN film is the same as that of the first AlN film, and the sputtering pressure of the second AlN film is the same as that of the first AlN film. The method can ensure good quality of the finally obtained AlN buffer layer and effectively improve the forming efficiency of the AlN buffer layer.
示例性地,第一靶间距为70mm~100mm,第二靶间距为40mm~70mm。Exemplarily, the first target distance is 70 mm to 100 mm, and the second target distance is 40 mm to 70 mm.
第一靶间距与第二靶间距为以上范围内时,所得到的第一AlN膜与第二AlN膜的质量会较好,且第一AlN膜与第二AlN膜沉积的效率也较高,可以有效减小发光二极管外延片的制备周期的同时提高发光二极管外延片的晶体质量。When the first target distance and the second target distance are within the above range, the quality of the obtained first AlN film and the second AlN film will be better, and the deposition efficiency of the first AlN film and the second AlN film will be higher, The preparation period of the epitaxial wafer of the light emitting diode can be effectively reduced while the crystal quality of the epitaxial wafer of the light emitting diode can be improved.
可选地,第一靶间距与第二靶间距之差的绝对值为20mm~50mm。Optionally, the absolute value of the difference between the first target distance and the second target distance is 20 mm to 50 mm.
第一靶间距与第二靶间距之差的绝对值在以上范围内,可以控制第一AlN膜与第二AlN膜的质量差距较小,可以保证最终得到的AlN缓冲层的质量,同时AlN缓冲层的生长效率也较高,AlN缓冲层的生长时间可以得到缩短。If the absolute value of the difference between the first target distance and the second target distance is within the above range, the quality gap between the first AlN film and the second AlN film can be controlled to be small, and the quality of the final AlN buffer layer can be guaranteed. The growth efficiency of the layer is also high, and the growth time of the AlN buffer layer can be shortened.
可选地,第一AlN膜的溅射时长为2~20s,第二AlN膜的溅射时长与第一AlN膜的溅射时长相等。Optionally, the sputtering duration of the first AlN film is 2-20s, and the sputtering duration of the second AlN film is equal to the sputtering duration of the first AlN film.
第一AlN膜的溅射时长为2~20s,第二AlN膜的溅射时长与第一AlN膜的溅射时长相等,可以有效提高第一AlN膜与第二AlN膜的质量的同时,提高生长速率。The sputtering duration of the first AlN film is 2-20s, and the sputtering duration of the second AlN film is equal to the sputtering duration of the first AlN film, which can effectively improve the quality of the first AlN film and the second AlN film, and improve the growth rate.
示例性地,第一AlN膜的厚度为0.1~5nm。Exemplarily, the thickness of the first AlN film is 0.1-5 nm.
第一AlN膜的厚度在以上范围,可以保证得到的第一AlN膜的质量较好,且可以良好过渡到第二AlN膜,保证第一AlN膜上生长的第二AlN膜也可以具有较为良好的质量,提高最终得到的AlN缓冲层的质量。The thickness of the first AlN film is in the above range, which can ensure that the quality of the first AlN film obtained is better, and can transition to the second AlN film well, so that the second AlN film grown on the first AlN film can also have a relatively good quality. improve the quality of the final AlN buffer layer.
可选地,第二AlN膜的厚度为2~20nm。Optionally, the thickness of the second AlN film is 2-20 nm.
第二AlN膜的厚度在以上范围,可以保证得到的第二AlN膜的质量较好,且在第二AlN膜上生长的第一AlN膜的质量也会比较好,提高最终得到的AlN缓冲层的质量。在第一AlN膜的厚度与第二AlN膜的厚度分别在以上范围内时,还可以保证第一AlN膜与第二AlN膜交替生长时,内部的应力可以抵消大部分,以提高最终得到的AlN缓冲层的质量。The thickness of the second AlN film is in the above range, which can ensure that the quality of the second AlN film obtained is better, and the quality of the first AlN film grown on the second AlN film will also be better, improving the final obtained AlN buffer layer. the quality of. When the thickness of the first AlN film and the thickness of the second AlN film are respectively in the above ranges, it can also be ensured that when the first AlN film and the second AlN film grow alternately, the internal stress can offset most of them, so as to improve the final obtained The quality of the AlN buffer layer.
需要说明的是,在交替溅射的过程中,实际上AlN缓冲层的厚度会缓慢增加,因此后续溅射时,虽然第一靶间距与第二靶间距没变,但靶材到AlN材料的距离实际上是有一定程度的减小的,因此在交替生长多次第一AlN膜与第二AlN膜之后,第一AlN膜与第二AlN膜的生长速率都会轻微提升,进一步减小第一AlN膜与第二AlN膜生长所需时间。而在第一AlN膜的厚度与第二AlN膜军具有一定的厚度的情况下,第一AlN膜与第二AlN膜的质量则不会受到溅射速度轻微提升的影响。It should be noted that in the process of alternate sputtering, the thickness of the AlN buffer layer will actually increase slowly. Therefore, in the subsequent sputtering, although the first target distance and the second target distance remain unchanged, the distance between the target material and the AlN material The distance actually decreases to a certain extent, so after alternately growing the first AlN film and the second AlN film multiple times, the growth rates of the first AlN film and the second AlN film will both increase slightly, further reducing the first AlN film. The time required for the growth of the AlN film and the second AlN film. However, when the thickness of the first AlN film and the second AlN film have a certain thickness, the quality of the first AlN film and the second AlN film will not be affected by a slight increase in sputtering speed.
可选地,第二AlN膜的厚度与第一AlN膜的厚度之比为5~20。Optionally, the ratio of the thickness of the second AlN film to the thickness of the first AlN film is 5-20.
第二AlN膜的厚度与第一AlN膜的厚度之比在以上范围内,最终得到的AlN缓冲层的质量较好。If the ratio of the thickness of the second AlN film to the thickness of the first AlN film is within the above range, the quality of the finally obtained AlN buffer layer is better.
在本公开所提供的一种实现方式中,步骤S203还可包括:In an implementation manner provided in the present disclosure, step S203 may further include:
溅射第一AlN膜之后,间隔20~100s,进行第二AlN膜的溅射。After the first AlN film is sputtered, the second AlN film is sputtered at an interval of 20 to 100 s.
溅射第一AlN膜之后,间隔以上时长再进行第二AlN膜的溅射,中间具有一定的时间可以用于调整磁控溅射装置中靶材的位置,并且这个时间内,第一AlN膜也有一定的时间释放内部应力,提高最终得到的AlN缓冲的质量。After the first AlN film is sputtered, the second AlN film is sputtered after an interval of more than a certain period of time can be used to adjust the position of the target in the magnetron sputtering device, and within this time, the first AlN film There is also time to release internal stresses, improving the quality of the resulting AlN buffer.
示例性地,第二AlN膜溅射完之后,也可以间隔20~100s,再进行第一AlN膜的溅射。同样可以提高第二AlN膜的质量,以提高AlN缓冲的质量。Exemplarily, after the second AlN film is sputtered, the first AlN film may be sputtered again at an interval of 20-100 s. It is also possible to increase the quality of the second AlN film to increase the quality of the AlN buffer.
可选地,在第一AlN膜与第二AlN膜的溅射过程中,磁控溅射装置中所通入的气体包括氩气、氮气与氧气。Optionally, during the sputtering process of the first AlN film and the second AlN film, the gas introduced into the magnetron sputtering device includes argon, nitrogen and oxygen.
第一AlN膜与第二AlN膜的溅射过程中通入以上气体,可以有效降低第一AlN膜与第二AlN膜的内部缺陷,提高最终得到的第一AlN膜与第二AlN膜的晶体质量。The above gas is passed into the sputtering process of the first AlN film and the second AlN film, which can effectively reduce the internal defects of the first AlN film and the second AlN film, and improve the crystallinity of the first AlN film and the second AlN film finally obtained. quality.
示例性地,在第一AlN膜与第二AlN膜的溅射过程中,磁控溅射装置中所通入的氩气流量为30~100sccm,氮气的流量为100~200sccm,氧气的流量为1~5sccm。能够得到质量较好的第一AlN膜与第二AlN膜。Exemplarily, during the sputtering process of the first AlN film and the second AlN film, the flow rate of argon gas fed into the magnetron sputtering device is 30-100 sccm, the flow rate of nitrogen gas is 100-200 sccm, and the flow rate of oxygen gas is 1~5 sccm. The first AlN film and the second AlN film with better quality can be obtained.
在本公开所提供的一种实现方式中,氩气流量为50sccm,氮气的流量为150sccm,氧气的流量为2sccm。能够得到质量较好的第一AlN膜与第二AlN膜。In an implementation manner provided in the present disclosure, the flow rate of the argon gas is 50 sccm, the flow rate of the nitrogen gas is 150 sccm, and the flow rate of the oxygen gas is 2 sccm. The first AlN film and the second AlN film with better quality can be obtained.
在本公开所提供的一种实现方式中,第一AlN膜的溅射次数与第二AlN膜的溅射次数之和可为3~10次。In an implementation manner provided by the present disclosure, the sum of the sputtering times of the first AlN film and the sputtering times of the second AlN film may be 3-10 times.
第一AlN膜的溅射次数与第二AlN膜的溅射次数之和为3~10次,能够保证最终得到的AlN缓冲层的质量较好。The sum of the sputtering times of the first AlN film and the sputtering times of the second AlN film is 3-10 times, which can ensure that the quality of the finally obtained AlN buffer layer is better.
在本公开所提供的一种实现方式中,第一AlN膜的溅射次数与第二AlN膜的溅射次数之和可为3。可以减小生长周期的同时提高AlN缓冲层的质量。In an implementation manner provided by the present disclosure, the sum of the sputtering times of the first AlN film and the sputtering times of the second AlN film may be three. The growth period can be reduced while improving the quality of the AlN buffer layer.
S204:对AlN缓冲层进行10~15min的热处理。S204: performing heat treatment on the AlN buffer layer for 10-15 minutes.
对生长得到的AlN缓冲层进行以上时长的热处理,可以去除AlN缓冲层上所残留的杂质等,提高AlN缓冲层的表面质量,以提高在AlN缓冲层上生长的外延材料的质量。The above-mentioned length of heat treatment on the grown AlN buffer layer can remove residual impurities on the AlN buffer layer, improve the surface quality of the AlN buffer layer, and improve the quality of the epitaxial material grown on the AlN buffer layer.
可选地,对AlN缓冲层进行热处理的温度为1100~1200℃。Optionally, the temperature for heat treatment of the AlN buffer layer is 1100-1200°C.
对AlN缓冲层进行热处理的温度为以上范围,可以有效去除杂质。The heat treatment temperature of the AlN buffer layer is in the above range, and impurities can be effectively removed.
示例性地,在氢气氛围下对AlN缓冲层进行热处理。可以有效去除杂质。Exemplarily, the AlN buffer layer is heat-treated in a hydrogen atmosphere. Can effectively remove impurities.
S205:在对AlN缓冲层上生长GaN缓冲层。S205: growing a GaN buffer layer on the AlN buffer layer.
示例性地,GaN缓冲层的生长温度可为530~560℃,压力可为200~500mtorr。得到的GaN缓冲层的质量较好。Exemplarily, the growth temperature of the GaN buffer layer may be 530-560° C., and the pressure may be 200-500 mtorr. The quality of the obtained GaN buffer layer is better.
S206:在GaN缓冲层上生长非掺杂GaN层。S206: growing a non-doped GaN layer on the GaN buffer layer.
非掺杂GaN层的厚度可为0.5~3um。The thickness of the non-doped GaN layer may be 0.5-3um.
示例性地,非掺杂GaN层的生长温度可为1000~1100℃,生长压力控制在100~300torr。得到的非掺杂GaN层的质量较好。Exemplarily, the growth temperature of the non-doped GaN layer may be 1000-1100° C., and the growth pressure may be controlled at 100-300 torr. The quality of the obtained undoped GaN layer is better.
S207:在非掺杂GaN层上生长n型GaN层。S207: growing an n-type GaN layer on the non-doped GaN layer.
可选地,n型GaN层的生长温度可为1000~1100℃,n型GaN层的生长压力可为100~300Torr。Optionally, the growth temperature of the n-type GaN layer may be 1000-1100° C., and the growth pressure of the n-type GaN layer may be 100-300 Torr.
可选地,n型GaN层的厚度可为0.5~3um。Optionally, the thickness of the n-type GaN layer may be 0.5-3um.
S208:在n型GaN层上生长多量子阱层。多量子阱层包括交替生长的阱层和GaN垒层。S208: growing multiple quantum well layers on the n-type GaN layer. The multiple quantum well layer includes alternately grown well layers and GaN barrier layers.
示例性地,阱层的生长温度可为700~830℃。GaN垒层的生长温度为800~960℃。能够得到质量较好的多量子阱层。Exemplarily, the growth temperature of the well layer may be 700-830°C. The growth temperature of the GaN barrier layer is 800-960°C. A multi-quantum well layer with better quality can be obtained.
S209:在多量子阱层上生长电子阻挡层。S209: growing an electron blocking layer on the multiple quantum well layer.
电子阻挡层可为AlGaN电子阻挡层,AlGaN电子阻挡层的生长温度可为800~1000℃,AlGaN电子阻挡层的生长压力可为100~300Torr。在此条件下生长得到的AlGaN电子阻挡层的质量较好,有利于提高发光二极管的发光效率。The electron blocking layer may be an AlGaN electron blocking layer, the growth temperature of the AlGaN electron blocking layer may be 800-1000° C., and the growth pressure of the AlGaN electron blocking layer may be 100-300 Torr. The quality of the AlGaN electron blocking layer grown under this condition is better, which is conducive to improving the luminous efficiency of the light emitting diode.
S210:在电子阻挡层上生长p型GaN层。S210: growing a p-type GaN layer on the electron blocking layer.
可选地,p型GaN层的生长压力可为200~600Torr,p型GaN层的生长温度可为800~1000℃。Optionally, the growth pressure of the p-type GaN layer may be 200-600 Torr, and the growth temperature of the p-type GaN layer may be 800-1000°C.
S211:在p型GaN层上生长p型接触层。S211: growing a p-type contact layer on the p-type GaN layer.
可选地,p型接触层的生长压力可为100~300Torr,p型接触层的生长温度可为800~1000℃。Optionally, the growth pressure of the p-type contact layer may be 100-300 Torr, and the growth temperature of the p-type contact layer may be 800-1000°C.
需要说明的是,图5中所示的具有AlN的发光二极管外延片的制备方法,相对图1中所示的发光二极管的制备方法,提供了一种更为详细的发光二极管外延片的生长方式。It should be noted that the preparation method of the LED epitaxial wafer with AlN shown in FIG. 5 provides a more detailed growth method of the LED epitaxial wafer compared with the preparation method of the LED shown in FIG. 1 .
需要说明的是,在本公开实施例中,采用VeecoK 465i or C4 or RB MOCVD(MetalOrganic Chemical Vapor Deposition,金属有机化合物化学气相沉淀)设备实现发光二极管的生长方法。采用高纯H2(氢气)或高纯N2(氮气)或高纯H2和高纯N2的混合气体作为载气,高纯NH3作为N源,三甲基镓(TMGa)及三乙基镓(TEGa)作为镓源,三甲基铟(TMIn)作为铟源,硅烷(SiH4)作为N型掺杂剂,三甲基铝(TMAl)作为铝源,二茂镁(CP2Mg)作为P型掺杂剂。It should be noted that, in the embodiments of the present disclosure, VeecoK 465i or C4 or RB MOCVD (MetalOrganic Chemical Vapor Deposition, metal organic compound chemical vapor deposition) equipment is used to realize the growth method of light emitting diodes. Use high-purity H 2 (hydrogen) or high-purity N 2 (nitrogen) or a mixture of high-purity H 2 and high-purity N 2 as carrier gas, high-purity NH 3 as N source, trimethylgallium (TMGa) and three Ethyl gallium (TEGa) as gallium source, trimethyl indium (TMIn) as indium source, silane (SiH4) as N-type dopant, trimethyl aluminum (TMAl) as aluminum source, dimagnesocene (CP 2 Mg ) as a P-type dopant.
执行完步骤S211后的发光二极管外延片的结构可参见图5。The structure of the light emitting diode epitaxial wafer after step S211 can be referred to FIG. 5 .
图5是本公开实施例提供的另一种发光二极管外延片的结构示意图,参考图5可知,在本公开提供的另一种实现方式中,发光二极管外延片可包括衬底1及生长在衬底1上的AlN缓冲层2、GaN缓冲层6、非掺杂GaN层7、n型GaN层3、多量子阱层4、电子阻挡层8、p型GaN层5及p型接触层9。FIG. 5 is a schematic structural view of another light-emitting diode epitaxial wafer provided by an embodiment of the present disclosure. Referring to FIG.
图5中所示的AlN缓冲层2的结构可参考图3中所示的AlN缓冲层2的结构,因此此处不再赘述。The structure of the
可选地,GaN缓冲层6的厚度可为10~30nm。能够减小n型GaN层与衬底1之间的晶格失配,保证外延层的晶体质量。Optionally, the GaN buffer layer 6 may have a thickness of 10-30 nm. The lattice mismatch between the n-type GaN layer and the
示例性地,非掺杂GaN层7的厚度可为1~3.5μm。此时得到的发光二极管外延片的质量较好。Exemplarily, the thickness of the non-doped GaN layer 7 may be 1-3.5 μm. The quality of the light emitting diode epitaxial wafer obtained at this time is relatively good.
可选地,n型GaN层3的掺杂元素可为Si,且Si元素的掺杂浓度可为1×1018~1×1019cm-3。n型GaN层3整体的质量较好。Optionally, the doping element of the n-
示例性地,n型GaN层3的厚度可为2~3μm。得到的n型GaN层整体的质量较好。Exemplarily, the thickness of the n-
可选地,多量子阱层4可包括交替层叠的阱层41与GaN垒层42。易于制备与获取。Optionally, the
可选地,电子阻挡层8中Al组分可为0.15~0.25。阻挡电子的效果较好。Optionally, the Al composition in the electron blocking layer 8 may be 0.15-0.25. The effect of blocking electrons is better.
可选地,p型GaN层5可掺Mg。Optionally, the p-
示例性地,p型接触层9的厚度可为15nm。Exemplarily, the thickness of the p-type contact layer 9 may be 15 nm.
需要说明的是,图5中所示的外延片结构相对图3中所示的外延片结构,在多量子阱层4与p型GaN层5之间增加了电子阻挡层8,在p型GaN层5上还生长有p型接触层9。得到的外延片的质量及发光效率会更好。It should be noted that, compared with the epitaxial wafer structure shown in FIG. 3, the epitaxial wafer structure shown in FIG. 5 has an electron blocking layer 8 added between the
以上所述,并非对本发明作任何形式上的限制,虽然本发明已通过实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。The above description does not limit the present invention in any form. Although the present invention has been disclosed above through the embodiments, it is not used to limit the present invention. When the technical content disclosed above can be used to make some changes or be modified into equivalent embodiments with equivalent changes, any simple modifications made to the above embodiments according to the technical essence of the present invention, Equivalent changes and modifications still fall within the scope of the technical solution of the present invention.
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