CN106409996A - Epitaxial growth method capable of improving LED chip property uniformity - Google Patents
Epitaxial growth method capable of improving LED chip property uniformity Download PDFInfo
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Abstract
Description
技术领域technical field
本申请涉及LED外延设计应用技术领域,具体地说,涉及一种改善LED芯片性能均匀性的外延生长方法。The present application relates to the technical field of LED epitaxial design application, in particular, to an epitaxial growth method for improving the performance uniformity of LED chips.
背景技术Background technique
目前LED(Light Emitting Diode,发光二极管)是一种固体照明,体积小、耗电量低使用寿命长高亮度、环保、坚固耐用等优点受到广大消费者认可,国内生产LED的规模也在逐步扩大。At present, LED (Light Emitting Diode, light-emitting diode) is a kind of solid-state lighting. Its advantages such as small size, low power consumption, long service life, high brightness, environmental protection, and durability are recognized by consumers, and the scale of domestic production of LEDs is gradually expanding. .
近年,直接带隙半导体材料GaN被广泛应用于发光二极管器件。利用直流磁控反应溅射设备再蓝宝石衬底上制备AlN薄膜,再利用金属有机化学气相沉淀(metal-organicchemical vapor deposition,MOCVD)可制备更高晶体质量的GaN基材料,这种溅射AlN生长GaN外延技术正在逐步取代传统的两步生长法(先在异质衬底上低温生长GaN、AlN、AlGaN等缓冲层经过高温退火后生长GaN、AlN、AlGaN等材料)。但由于蓝宝石和AlN材料存在较大的晶格失配和热失配,导致该技术生长的外延片片内性能均匀性较差,如波长、厚度、亮度等,严重困扰技术的推广。In recent years, the direct bandgap semiconductor material GaN has been widely used in light-emitting diode devices. Using DC magnetron reactive sputtering equipment to prepare AlN thin films on sapphire substrates, and then using metal-organic chemical vapor deposition (metal-organic chemical vapor deposition, MOCVD) can prepare GaN-based materials with higher crystal quality. This sputtering AlN growth GaN epitaxy technology is gradually replacing the traditional two-step growth method (first grow GaN, AlN, AlGaN and other buffer layers on heterogeneous substrates at low temperature, and then grow GaN, AlN, AlGaN and other materials after high-temperature annealing). However, due to the large lattice mismatch and thermal mismatch between sapphire and AlN materials, the epitaxial wafers grown by this technology have poor uniformity in performance, such as wavelength, thickness, brightness, etc., which seriously plagues the promotion of the technology.
发明内容Contents of the invention
有鉴于此,本申请所要解决的技术问题是提供了一种改善LED芯片性能均匀性的外延生长方法,通过引入应力释放层,能明显弱化晶格失配和热失配带来的负面效应,改善了外延片片内波长、厚度、亮度的均匀性,有利于溅射AlN生长GaN外延技术的广泛推广。In view of this, the technical problem to be solved in this application is to provide an epitaxial growth method to improve the performance uniformity of the LED chip. By introducing a stress release layer, the negative effects caused by lattice mismatch and thermal mismatch can be significantly weakened. The uniformity of wavelength, thickness and brightness in the epitaxial wafer is improved, which is conducive to the wide promotion of sputtering AlN growth GaN epitaxial technology.
为了解决上述技术问题,本申请有如下技术方案:In order to solve the above technical problems, the application has the following technical solutions:
一种改善LED芯片性能均匀性的外延生长方法,其特征在于,依次包括:处理图形化蓝宝石衬底、生长应力释放层、生长非掺杂GaN层、生长掺杂Si的N型GaN层、生长多量子阱有源层、生长电子阻挡层、生长掺杂Mg的P型GaN层、降温冷却,其中,An epitaxial growth method for improving the performance uniformity of an LED chip, characterized in that it sequentially includes: processing a patterned sapphire substrate, growing a stress release layer, growing a non-doped GaN layer, growing a Si-doped N-type GaN layer, growing Multi-quantum well active layer, growing electron blocking layer, growing Mg-doped P-type GaN layer, cooling down, wherein,
所述处理图像化蓝宝石衬底,为:利用直流磁控反应溅射设备将所述蓝宝石衬底温度加热到500℃-700℃,通入Ar、N2和O2,用200V~300V的偏压冲击铝靶在所述蓝宝石衬底表面上溅射10nm~200nm厚的AlN薄膜;The process of processing the imaged sapphire substrate is as follows: using DC magnetron reactive sputtering equipment to heat the temperature of the sapphire substrate to 500°C-700°C, injecting Ar, N 2 and O 2 , using a 200V-300V bias Sputtering an AlN film with a thickness of 10nm to 200nm on the surface of the sapphire substrate by pressure impacting an aluminum target;
所述生长应力释放层,为:将溅射好所述AlN薄膜的蓝宝石衬底放入MOCVD反应腔,升高温度到500℃-1000℃,保持反应腔压力为150mbar~600mbar,生长厚度为10nm-200nm的应力释放层,所述应力释放层为GaN基材料,具体为:非掺杂的GaN、掺Si的GaN、或掺Mg的GaN、AlGaN、InGAN、AlInGaN。The growth of the stress release layer is as follows: put the sapphire substrate sputtered with the AlN thin film into the MOCVD reaction chamber, raise the temperature to 500°C-1000°C, keep the pressure of the reaction chamber at 150mbar-600mbar, and grow the thickness to 10nm - a 200nm stress release layer, the stress release layer is a GaN-based material, specifically: non-doped GaN, Si-doped GaN, or Mg-doped GaN, AlGaN, InGAN, AlInGaN.
优选地,其中:Preferably, where:
所述掺Si的GaN中,Si掺杂浓度为0atoms/cm3-2E+19atoms/cm3;In the Si-doped GaN, the Si doping concentration is 0 atoms/cm 3 -2E+19 atoms/cm 3 ;
所述掺Mg的GaN、AlGaN、InGAN、AlInGaN中,Mg掺杂浓度为0atoms/cm3-1+E21atoms/cm3。In the Mg-doped GaN, AlGaN, InGAN, AlInGaN, the Mg doping concentration is 0 atoms/cm 3 −1+E21 atoms/cm 3 .
优选地,其中:Preferably, where:
所述生长非掺杂GaN层,为:升高温度到1000℃~1200℃,保持反应腔压力为150mbar~600mbar,生长厚度为1μm~4μm的非掺杂GaN层。The growth of the non-doped GaN layer includes: increasing the temperature to 1000° C. to 1200° C., keeping the reaction chamber pressure at 150 mbar to 600 mbar, and growing the non-doped GaN layer with a thickness of 1 μm to 4 μm.
优选地,其中:Preferably, where:
所述生长掺杂Si的N型GaN层,为:保持反应腔温度为1000℃~1200℃,压力为150mbar~600mbar,在150mbar~300mbar的氢气气氛下生长厚度为1μm~4μm的N型GaN层,其中,Si掺杂浓度为5E+18atoms/cm3~2E+19atoms/cm3。The growth of the Si-doped N-type GaN layer is: keep the temperature of the reaction chamber at 1000°C-1200°C, the pressure at 150mbar-600mbar, and grow the N-type GaN layer with a thickness of 1μm-4μm under a hydrogen atmosphere of 150mbar-300mbar , wherein the Si doping concentration is 5E+18 atoms/cm 3 -2E+19 atoms/cm 3 .
优选地,其中:Preferably, where:
所述生长多量子阱有源层,为:The growing multiple quantum well active layer is:
降低温度到700℃~750℃,保持反应腔压力为300mbar~400mbar,在氮气气氛下,生长厚度为2.5nm-3.5nm的InxGa(1-x)N势阱层,其中,x=0.15~0.25,In掺杂浓度为1E+20atoms/cm3~5E+20atoms/cm3;Lower the temperature to 700°C-750°C, keep the reaction chamber pressure at 300mbar-400mbar, and grow an In x Ga (1 -x)N potential well layer with a thickness of 2.5nm-3.5nm in a nitrogen atmosphere, where x=0.15 ~0.25, In doping concentration is 1E+20atoms/cm 3 ~5E+20atoms/cm 3 ;
然后升高温度至800℃~850℃,保持反应腔压力不变,生长厚度为8nm~12nm的GaN势垒层;Then raise the temperature to 800°C-850°C, keep the pressure of the reaction chamber constant, and grow a GaN barrier layer with a thickness of 8nm-12nm;
交替生长所述势阱层和所述势垒层,生长周期为6~15,制得InxGa(1-x)N/GaN多量子阱有源层。The potential well layer and the potential barrier layer are alternately grown with a growth period of 6-15 to prepare an InxGa (1 - x )N/GaN multi-quantum well active layer.
优选地,其中:Preferably, where:
所述生长电子阻挡层,为:升高温度到800℃~900℃,在200mbar~400mbar的反应腔压力下,生长厚度为10nm~200nm的P型AlyGa(1-y)N电子阻挡层,其中,y=0.1~0.3,Al掺杂浓度为1E+20atoms/cm3~3E+20atoms/cm3,Mg掺杂浓度为5E+18atoms/cm3~1E+19atoms/cm3。The growth of the electron blocking layer is: increasing the temperature to 800°C-900°C, and growing a P-type Al y Ga (1-y) N electron blocking layer with a thickness of 10nm-200nm under the reaction chamber pressure of 200mbar-400mbar , wherein, y=0.1˜0.3, Al doping concentration is 1E+20atoms/cm 3 ˜3E+20atoms/cm 3 , Mg doping concentration is 5E+18atoms/cm 3 ˜1E+19atoms/cm 3 .
优选地,其中:Preferably, where:
所述生长掺杂Mg的P型GaN层,为:升高温度到930℃~950℃,在200mbar~600mbar的反应腔压力下,生长30nm~300nm的P型GaN层,其中,Mg掺杂浓度为1E+19atoms/cm3~1E+20atoms/cm3。The growth of the P-type GaN layer doped with Mg is as follows: increasing the temperature to 930°C-950°C, and growing a P-type GaN layer of 30nm-300nm under the reaction chamber pressure of 200mbar-600mbar, wherein the Mg doping concentration is It is 1E+19 atoms/cm 3 to 1E+20 atoms/cm 3 .
优选地,其中:Preferably, where:
所述降温冷却,为:降低温度至700℃~800℃,进行炉内退火20min~30min,接着冷却至室温。The temperature-lowering cooling includes: lowering the temperature to 700° C. to 800° C., annealing in a furnace for 20 minutes to 30 minutes, and then cooling to room temperature.
与现有技术相比,本申请所述的方法,达到了如下效果:Compared with the prior art, the method described in this application has achieved the following effects:
(1)本发明改善LED芯片性能均匀性的外延生长方法,与传统方法相比,加入了应力释放层,该应力释放层具有比高温GaN更好的松弛度,能很好释放GaN与AlN模板直接的晶格应力,改善了外延生长时wafer的翘曲,使片内温度变得更加均匀,即提高了外延生长时片内长速的一致性,因此提高了GaN材料的厚度均匀性。(1) The epitaxial growth method of the present invention to improve the performance uniformity of the LED chip, compared with the traditional method, adds a stress release layer, the stress release layer has better relaxation than high-temperature GaN, and can release GaN and AlN templates well The direct lattice stress improves the warpage of the wafer during epitaxial growth and makes the temperature inside the chip more uniform, that is, improves the consistency of the growth rate in the chip during epitaxial growth, thus improving the thickness uniformity of GaN materials.
(2)本发明改善LED芯片性能均匀性的外延生长方法,加入的应力释放层很好的释放了GaN材料因晶格失配带来的应力,使wafer在生长量子阱时的片内温度变均匀,因而得到较高的波长一致性。(2) The epitaxial growth method of the present invention improves the performance uniformity of the LED chip, and the added stress release layer well releases the stress caused by the lattice mismatch of the GaN material, so that the internal temperature of the wafer when growing the quantum well changes. Uniform, thus obtaining higher wavelength consistency.
(3)本发明改善LED芯片性能均匀性的外延生长方法,加入应力释放层后,wafer表面温度变得均匀,使外延在生长每个结构时的一致性都得到提高,发光强度自然也具有更好的均匀性;另外,波长的均匀性的提高表明 样品A的量子阱区域InGaN分布更均匀,有利于提高外延片的亮度及其均匀性。(3) The epitaxial growth method of the present invention improves the performance uniformity of the LED chip. After adding the stress release layer, the surface temperature of the wafer becomes uniform, so that the consistency of the epitaxial growth of each structure is improved, and the luminous intensity is naturally higher. Good uniformity; in addition, the increase in the uniformity of the wavelength indicates that the distribution of InGaN in the quantum well region of sample A is more uniform, which is conducive to improving the brightness and uniformity of the epitaxial wafer.
附图说明Description of drawings
此处所说明的附图用来提供对本申请的进一步理解,构成本申请的一部分,本申请的示意性实施例及其说明用于解释本申请,并不构成对本申请的不当限定。在附图中:The drawings described here are used to provide a further understanding of the application and constitute a part of the application. The schematic embodiments and descriptions of the application are used to explain the application and do not constitute an improper limitation to the application. In the attached picture:
图1为本发明改善LED芯片性能均匀性的外延生长方法的流程图;Fig. 1 is the flow chart of the epitaxial growth method of improving LED chip performance uniformity of the present invention;
图2为本发明中LED外延层的结构示意图;Fig. 2 is the structural representation of LED epitaxial layer in the present invention;
图3为对比实施例中LED外延层的结构示意图;Fig. 3 is the structural representation of LED epitaxial layer in comparative example;
图4为使用PL测试样品A和样品B的GaN基材料厚度的分布对比图;Fig. 4 is a comparison diagram of the distribution of GaN-based material thickness of sample A and sample B using PL;
图5为使用PL测试样品A和样品B波长的分布对比图;Figure 5 is a comparison chart of the wavelength distribution of sample A and sample B using PL;
图6为使用PL测试样品A和样品B的发光强度的分布对比图;Figure 6 is a comparison diagram of the distribution of luminous intensities of sample A and sample B using PL;
其中,1、图形化蓝宝石衬底,2、溅射A1N缓冲层,3、u型GaN层,4、n型GaN层,5、多量子阱有源层,6、P型AlGaN层,7、P型GaN层,8、应力释放层。Among them, 1. patterned sapphire substrate, 2. sputtered AlN buffer layer, 3. u-type GaN layer, 4. n-type GaN layer, 5. multi-quantum well active layer, 6. p-type AlGaN layer, 7. P-type GaN layer, 8. Stress release layer.
具体实施方式detailed description
如在说明书及权利要求当中使用了某些词汇来指称特定组件。本领域技术人员应可理解,硬件制造商可能会用不同名词来称呼同一个组件。本说明书及权利要求并不以名称的差异来作为区分组件的方式,而是以组件在功能上的差异来作为区分的准则。如在通篇说明书及权利要求当中所提及的“包含”为一开放式用语,故应解释成“包含但不限定于”。“大致”是指在可接收的误差范围内,本领域技术人员能够在一定误差范围内解决所述技术问题,基本达到所述技术效果。此外,“耦接”一词在此包含任何直接及间接的电性耦接手段。因此,若文中描述一第一装置耦接于一第二装置,则代表所述第一装置可直接电性耦接于所述第二装置,或通过其他装置或耦接手段间接地电性耦接至所述第二装置。说明书后续描述为实施本申请的较佳实施方式,然 所述描述乃以说明本申请的一般原则为目的,并非用以限定本申请的范围。本申请的保护范围当视所附权利要求所界定者为准。Certain terms are used, for example, in the description and claims to refer to particular components. Those skilled in the art should understand that hardware manufacturers may use different terms to refer to the same component. The specification and claims do not use the difference in name as a way to distinguish components, but use the difference in function of components as a criterion for distinguishing. As mentioned throughout the specification and claims, "comprising" is an open term, so it should be interpreted as "including but not limited to". "Approximately" means that within an acceptable error range, those skilled in the art can solve the technical problem within a certain error range and basically achieve the technical effect. In addition, the term "coupled" herein includes any direct and indirect electrical coupling means. Therefore, if it is described that a first device is coupled to a second device, it means that the first device may be directly electrically coupled to the second device, or indirectly electrically coupled through other devices or coupling means. connected to the second device. The subsequent description of the specification is a preferred implementation mode for implementing the application, but the description is for the purpose of illustrating the general principles of the application, and is not intended to limit the scope of the application. The scope of protection of the present application should be defined by the appended claims.
实施例1Example 1
本发明运用型号为iTop A230的RMS设备在PSS上溅射AlN薄膜作为GaN外延生长的缓冲层,其载气为高纯氮气(N2)、高纯氦气(Ar)及少量高纯氧气(O2),靶材为高纯金属铝(Al),直流溅射电压为200-300V。采用veeco公司型号为K465i的MOCVD设备来生长高亮度GaN基LED外延片,以高纯氢气(H2)、高纯氮气(N2)作为载气,高纯氨气(NH3)作为N源,金属有机源三甲基镓(TMGa)和三乙基镓(TEGa)作为镓源,三甲基铟(TMIn)作为铟源,三甲基铝(TMAl)作为铝源,硅烷(SiH4)作为N型掺杂剂,二茂镁(CP2Mg)作为P型掺杂剂。The present invention uses the RMS equipment model iTop A230 to sputter AlN film on PSS as the buffer layer of GaN epitaxial growth, and its carrier gas is high-purity nitrogen (N 2 ), high-purity helium (Ar) and a small amount of high-purity oxygen ( O 2 ), the target material is high-purity metal aluminum (Al), and the DC sputtering voltage is 200-300V. Use veeco company model K465i MOCVD equipment to grow high-brightness GaN-based LED epitaxial wafers, use high-purity hydrogen (H 2 ), high-purity nitrogen (N 2 ) as carrier gas, and high-purity ammonia (NH 3 ) as N source , metal-organic sources trimethylgallium (TMGa) and triethylgallium (TEGa) as gallium source, trimethylindium (TMIn) as indium source, trimethylaluminum (TMAl) as aluminum source, silane (SiH4) as The N-type dopant, magnesium dicene (CP2Mg) is used as the P-type dopant.
本发明所提供的改善LED芯片性能均匀性的外延生长方法,依次包括:处理图形化蓝宝石衬底、生长应力释放层、生长非掺杂GaN层、生长掺杂Si的N型GaN层、生长多量子阱有源层、生长电子阻挡层、生长掺杂Mg的P型GaN层、降温冷却,其中,The epitaxial growth method for improving the performance uniformity of the LED chip provided by the present invention sequentially includes: processing a patterned sapphire substrate, growing a stress release layer, growing a non-doped GaN layer, growing an N-type GaN layer doped with Si, growing a poly Quantum well active layer, growing electron blocking layer, growing Mg-doped P-type GaN layer, cooling down, wherein,
所述处理图像化蓝宝石衬底,为:利用直流磁控反应溅射设备将所述蓝宝石衬底温度加热到500℃-700℃,通入Ar、N2和O2,用200V~300V的偏压冲击铝靶在所述蓝宝石衬底表面上溅射10nm~200nm厚的AlN薄膜;The process of processing the imaged sapphire substrate is as follows: using DC magnetron reactive sputtering equipment to heat the temperature of the sapphire substrate to 500°C-700°C, injecting Ar, N 2 and O 2 , using a 200V-300V bias Sputtering an AlN film with a thickness of 10nm to 200nm on the surface of the sapphire substrate by pressure impacting an aluminum target;
所述生长应力释放层,为:将溅射好所述AlN薄膜的蓝宝石衬底放入MOCVD反应腔,升高温度到500℃-1000℃,保持反应腔压力为150mbar~600mbar,生长厚度为10nm-200nm的应力释放层,所述应力释放层为GaN基材料,具体为:非掺杂的GaN、掺Si的GaN、或掺Mg的GaN、AlGaN、InGAN、AlInGaN。The growth of the stress release layer is as follows: put the sapphire substrate sputtered with the AlN thin film into the MOCVD reaction chamber, raise the temperature to 500°C-1000°C, keep the pressure of the reaction chamber at 150mbar-600mbar, and grow the thickness to 10nm - a 200nm stress release layer, the stress release layer is a GaN-based material, specifically: non-doped GaN, Si-doped GaN, or Mg-doped GaN, AlGaN, InGAN, AlInGaN.
上述掺杂Si的GaN中,Si掺杂浓度为0-2E+19atoms/cm3;掺Mg的GaN、AlGaN、InGAN、AlInGaN中,Mg掺杂浓度为0-1+E21atoms/cm3。In the aforementioned Si-doped GaN, the Si doping concentration is 0-2E+19 atoms/cm 3 ; in the Mg-doped GaN, AlGaN, InGAN, AlInGaN, the Mg doping concentration is 0-1+E21 atoms/cm 3 .
本发通过的应力释放层,能明显弱化晶格失配和热失配带来的负面效应,改善了外延片片内波长、厚度、亮度的均匀性,有利于溅射AlN生长GaN外延技术的广泛推广。The stress release layer adopted by the present invention can significantly weaken the negative effects caused by lattice mismatch and thermal mismatch, improve the uniformity of wavelength, thickness, and brightness in the epitaxial wafer, and is conducive to the development of sputtering AlN growth GaN epitaxy technology Promote widely.
实施例2Example 2
以下提供本发明的改善LED芯片性能均匀性的外延生长方法的应用实施例,其外延结构参见图2,生长方法参见图1。运用型号为iTop A230的RMS设备在PSS上溅射AlN薄膜作为GaN外延生长的缓冲层,其载气为高纯氮气(N2)、高纯氦气(Ar)及少量高纯氧气(O2),靶材为高纯金属铝(Al),直流溅射电压为200-300V。采用veeco公司型号为K465i的MOCVD设备来生长高亮度GaN基LED外延片,以高纯氢气(H2)、高纯氮气(N2)作为载气,高纯氨气(NH3)作为N源,金属有机源三甲基镓(TMGa)和三乙基镓(TEGa)作为镓源,三甲基铟(TMIn)作为铟源,三甲基铝(TMAl)作为铝源,硅烷(SiH4)作为N型掺杂剂,二茂镁(CP2Mg)作为P型掺杂剂。具体生长方式如下:The application examples of the epitaxial growth method for improving LED chip performance uniformity of the present invention are provided below, the epitaxial structure is shown in FIG. 2 , and the growth method is shown in FIG. 1 . The AlN thin film was sputtered on the PSS by RMS equipment model iTop A230 as a buffer layer for GaN epitaxial growth, and the carrier gas was high-purity nitrogen (N 2 ), high-purity helium (Ar) and a small amount of high-purity oxygen (O 2 ), the target material is high-purity metal aluminum (Al), and the DC sputtering voltage is 200-300V. Use veeco company model K465i MOCVD equipment to grow high-brightness GaN-based LED epitaxial wafers, use high-purity hydrogen (H 2 ), high-purity nitrogen (N 2 ) as carrier gas, and high-purity ammonia (NH 3 ) as N source , metal-organic sources trimethylgallium (TMGa) and triethylgallium (TEGa) as gallium source, trimethylindium (TMIn) as indium source, trimethylaluminum (TMAl) as aluminum source, silane (SiH4) as The N-type dopant, magnesium dicene (CP2Mg) is used as the P-type dopant. The specific growth method is as follows:
步骤101、处理图形化蓝宝石衬底:Step 101, processing the patterned sapphire substrate:
利用直流磁控反应溅射设备将所述蓝宝石衬底温度加热到500℃-700℃,通入Ar、N2和O2,用200V~300V的偏压冲击铝靶在所述蓝宝石衬底表面上溅射10nm~200nm厚的AlN薄膜。Use DC magnetron reactive sputtering equipment to heat the temperature of the sapphire substrate to 500°C-700°C, pass through Ar, N 2 and O 2 , and impact the aluminum target on the surface of the sapphire substrate with a bias voltage of 200V-300V AlN film with a thickness of 10nm-200nm is sputtered on top.
步骤102、生长应力释放层:Step 102, growing a stress release layer:
将溅射好所述AlN薄膜的蓝宝石衬底放入MOCVD反应腔,升高温度到500℃-1000℃,保持反应腔压力为150mbar~600mbar,生长厚度为10nm-200nm的应力释放层,所述应力释放层为GaN基材料,具体可为:非掺杂的GaN、掺Si的GaN、或掺Mg的GaN、AlGaN、InGAN、AlInGaN。上述掺杂Si的GaN中,Si掺杂浓度为0-2E+19atoms/cm3;掺Mg的GaN、AlGaN、InGAN、AlInGaN中,Mg掺杂浓度为0-1+E21atoms/cm3。Put the sapphire substrate sputtered with the AlN thin film into the MOCVD reaction chamber, raise the temperature to 500°C-1000°C, keep the reaction chamber pressure at 150mbar-600mbar, and grow a stress release layer with a thickness of 10nm-200nm, the The stress release layer is a GaN-based material, specifically: non-doped GaN, Si-doped GaN, or Mg-doped GaN, AlGaN, InGAN, AlInGaN. In the aforementioned Si-doped GaN, the Si doping concentration is 0-2E+19 atoms/cm 3 ; in the Mg-doped GaN, AlGaN, InGAN, AlInGaN, the Mg doping concentration is 0-1+E21 atoms/cm 3 .
步骤103、生长非掺杂GaN层:Step 103, growing a non-doped GaN layer:
升高温度到1000℃~1200℃,保持反应腔压力为150mbar~600mbar,生长厚度为1μm~4μm的非掺杂GaN层。The temperature is raised to 1000° C. to 1200° C., the pressure of the reaction chamber is maintained at 150 mbar to 600 mbar, and a non-doped GaN layer with a thickness of 1 μm to 4 μm is grown.
步骤104、生长掺杂Si的N型GaN层:Step 104, growing an N-type GaN layer doped with Si:
保持反应腔温度为1000℃~1200℃,压力为150mbar~600mbar,在150mbar~300mbar的氢气气氛下生长厚度为1μm~4μm的N型GaN层,其中,Si掺杂浓度为5E+18atoms/cm3~2E+19atoms/cm3。Keep the temperature of the reaction chamber at 1000°C-1200°C, the pressure at 150mbar-600mbar, and grow an N-type GaN layer with a thickness of 1μm-4μm in a hydrogen atmosphere of 150mbar-300mbar, wherein the Si doping concentration is 5E+18atoms/cm 3 ~2E+19 atoms/cm 3 .
本申请中,5E18代表5乘以10的18次方也就是5*1018,以此类推,atoms/cm3为掺杂浓度单位,下同。In this application, 5E18 represents 5 times 10 to the 18th power, that is, 5*10 18 , and so on, atoms/cm 3 is the unit of doping concentration, the same below.
步骤105、生长多量子阱有源层:Step 105, growing the multi-quantum well active layer:
降低温度到700℃~750℃,保持反应腔压力为300mbar~400mbar,在氮气气氛下,生长厚度为2.5nm-3.5nm的InxGa(1-x)N势阱层,其中,x=0.15~0.25,In掺杂浓度为1E+20atoms/cm3~5E+20atoms/cm3;Lower the temperature to 700°C-750°C, keep the reaction chamber pressure at 300mbar-400mbar, and grow an In x Ga (1 -x)N potential well layer with a thickness of 2.5nm-3.5nm in a nitrogen atmosphere, where x=0.15 ~0.25, In doping concentration is 1E+20atoms/cm 3 ~5E+20atoms/cm 3 ;
然后升高温度至800℃~850℃,保持反应腔压力不变,生长厚度为8nm~12nm的GaN势垒层;Then raise the temperature to 800°C-850°C, keep the pressure of the reaction chamber constant, and grow a GaN barrier layer with a thickness of 8nm-12nm;
交替生长所述势阱层和所述势垒层,生长周期为6~15,制得InxGa(1-x)N/GaN多量子阱有源层。The potential well layer and the potential barrier layer are alternately grown with a growth period of 6-15 to prepare an In x Ga (1-x) N/GaN multi-quantum well active layer.
步骤106、生长电子阻挡层:Step 106, growing an electron blocking layer:
升高温度到800℃~900℃,在200mbar~400mbar的反应腔压力下,生长厚度为10nm~200nm的P型AlyGa(1-y)N电子阻挡层,其中,y=0.1~0.3,Al掺杂浓度为1E+20atoms/cm3~3E+20atoms/cm3,Mg掺杂浓度为5E+18atoms/cm3~1E+19atoms/cm3。raising the temperature to 800°C to 900°C, and growing a P-type Al y Ga (1-y) N electron blocking layer with a thickness of 10nm to 200nm under a reaction chamber pressure of 200mbar to 400mbar, where y=0.1 to 0.3, Al doping concentration is 1E+20atoms/cm 3 -3E+20atoms/cm 3 , and Mg doping concentration is 5E+18atoms/cm 3 -1E+19atoms/cm 3 .
步骤107、生长掺杂Mg的P型GaN层:Step 107, growing a P-type GaN layer doped with Mg:
升高温度到930℃~950℃,在200mbar~600mbar的反应腔压力下,生长30nm~300nm的P型GaN层,其中,Mg掺杂浓度为1E+19atoms/cm3~1E+20atoms/cm3。Raise the temperature to 930°C-950°C, and grow a P-type GaN layer of 30nm-300nm under the reaction chamber pressure of 200mbar-600mbar, wherein the Mg doping concentration is 1E+19atoms/cm 3 ~1E+20atoms/cm 3 .
步骤108、降温冷却:Step 108, cooling down:
降低温度至700℃~800℃,进行炉内退火20min~30min,接着冷却至室温。Lower the temperature to 700°C to 800°C, anneal in the furnace for 20min to 30min, and then cool to room temperature.
实施例3Example 3
以下提供一种常规GaN基LED器件外延生长方法作为本发明的对比实施例。A conventional GaN-based LED device epitaxial growth method is provided below as a comparative example of the present invention.
常规LED外延的生长方法为(外延层结构参见图3):The growth method of conventional LED epitaxy is (refer to Figure 3 for the epitaxial layer structure):
1、利用直流磁控反应溅射设备将PSS温度加热到500℃-700℃左右,通入氦气(Ar)、氮气(N2)和氧气(O2),用200V~300V的偏压冲击铝靶在PSS表面上溅射10nm~200nm厚的AlN薄膜。1. Use DC magnetron reactive sputtering equipment to heat the PSS temperature to about 500°C-700°C, feed helium (Ar), nitrogen (N 2 ) and oxygen (O 2 ), and impact with a bias voltage of 200V-300V The aluminum target sputters a 10nm-200nm thick AlN film on the surface of the PSS.
2、将溅射好AlN薄膜的PSS衬底放入MOCVD反应腔,升高温度到1000℃~1200℃,降低压力到150mbar~600mbar,通入NH3防止AlN薄膜分解。2. Put the PSS substrate sputtered with AlN film into the MOCVD reaction chamber, raise the temperature to 1000°C-1200°C, reduce the pressure to 150mbar-600mbar, and feed NH 3 to prevent the AlN film from decomposing.
3、保持温度在1000℃~1200℃,在150mbar~600mbar的压力下,生长厚度为1μm~4μm的非掺杂GaN层。3. Maintaining the temperature at 1000° C. to 1200° C. and growing a non-doped GaN layer with a thickness of 1 μm to 4 μm under a pressure of 150 mbar to 600 mbar.
4、维持反应腔的温度和压力,在150mbar~300mbar的氢气气氛下生长厚度为1μm~4μm的N型GaN层,Si掺杂浓度为5E+18atoms/cm3~2E+19atoms/cm3。4. Maintain the temperature and pressure of the reaction chamber, grow an N-type GaN layer with a thickness of 1 μm to 4 μm in a hydrogen atmosphere of 150 mbar to 300 mbar, and a Si doping concentration of 5E+18atoms/cm 3 to 2E+19atoms/cm 3 .
5、降温到700℃~750℃,在300mbar~400mbar的氮气气氛下生长厚度为2.5nm-3.5nm的InxGa(1-x)N(x=0.15~0.25)势阱层,In掺杂浓度为1E+20atoms/cm3~5E+20atoms/cm3;然后升高温度至800℃~850℃,压力不变,生长厚度为8nm~12nm的GaN势垒层;交替生长势阱层和势垒层6~15周期,制得InxGa(1-x)N/GaN多量子阱有源层。5. Lower the temperature to 700°C-750°C, and grow In x Ga (1-x) N (x=0.15-0.25) potential well layer with a thickness of 2.5nm-3.5nm under a nitrogen atmosphere of 300mbar-400mbar, and In doping The concentration is 1E+20atoms/cm 3 ~5E+20atoms/cm 3 ; then raise the temperature to 800°C~850°C, keep the pressure constant, and grow a GaN barrier layer with a thickness of 8nm~12nm; alternately grow potential well layers and potential The barrier layer has 6-15 periods, and the In x Ga (1-x) N/GaN multi-quantum well active layer is prepared.
6、升温到800℃~900℃,在200mbar~400mbar的压力下生长10nm~200nm的P型AlyGa(1-y)N(y=0.1~0.3)电子阻挡层,Al掺杂浓度为1E+20atoms/cm3~3E+20atoms/cm3,Mg掺杂浓度为5E+18atoms/cm3~1E+19atoms/cm3。6. Raise the temperature to 800°C~900°C, and grow a P-type Al y Ga (1-y) N (y=0.1~0.3) electron blocking layer of 10nm~200nm under the pressure of 200mbar~400mbar, and the Al doping concentration is 1E +20 atoms/cm 3 -3E+20 atoms/cm 3 , Mg doping concentration is 5E+ 18 atoms/cm 3 -1E+19 atoms/cm 3 .
7、升温到930℃~950℃,在200mbar~600mbar的压力下生长30nm~300nm的P型GaN层,Mg掺杂浓度为1E+19atoms/cm3~1E+20atoms/cm3。7. Raise the temperature to 930°C-950°C, grow a P-type GaN layer of 30nm-300nm under the pressure of 200mbar-600mbar, and the Mg doping concentration is 1E+19atoms/cm 3 -1E+20atoms/cm 3 .
8、最后降温至700℃~800℃,进行炉内退火20~30分钟,接着冷却至室温。8. Finally, lower the temperature to 700°C to 800°C, anneal in the furnace for 20 to 30 minutes, and then cool to room temperature.
在同一机台上,根据本专利描述的方法制备外延片样品A,其外延结构参见图2,根据常规的LED的生长方法(对比实施例的方法)制备样品B,其外延结构参见图3。On the same machine, epitaxial wafer sample A was prepared according to the method described in this patent, its epitaxial structure is shown in Figure 2, and sample B was prepared according to the conventional LED growth method (the method of the comparative example), and its epitaxial structure was shown in Figure 3.
图2和图3分别是本申请和对比实施例中LED外延结构图,样品A和样品B外延生长方法参数不同点在于图2中的应力释放层,即本发明在溅射A1N缓冲层和非掺杂GaN之间插入厚度为10nm-200nm的应力释放层。Fig. 2 and Fig. 3 are LED epitaxial structure diagrams in the present application and comparative examples respectively, and the difference between sample A and sample B epitaxial growth method parameters lies in the stress release layer in Fig. 2, namely the present invention sputters AlN buffer layer and A stress release layer with a thickness of 10nm-200nm is inserted between the doped GaN.
表1是样品A和样品B测试PL(光致发光测试仪)后,GaN材料的厚度、波长、发光强度及标准偏差(Std Dev,Standard Deviation)的对照表。很显然,本申请在加入应力释放层后,相比样品B而言,样品A外延片厚度的标准偏差、波长的标准偏差和光强的标准偏差都明显减小,也就是说外延片的厚度、波长、发光强度具有更好的均匀性,对外延片制作成芯片后产品的良率提升具有很大帮助。Table 1 is a comparison table of thickness, wavelength, luminous intensity and standard deviation (Std Dev, Standard Deviation) of GaN material after sample A and sample B are tested by PL (photoluminescence tester). Obviously, after adding the stress release layer in the present application, compared with sample B, the standard deviation of the thickness of the epitaxial wafer of sample A, the standard deviation of the wavelength and the standard deviation of the light intensity are all significantly reduced, that is to say, the thickness of the epitaxial wafer , wavelength, and luminous intensity have better uniformity, and it is of great help to improve the yield rate of the product after the epitaxial wafer is made into a chip.
表1外延片样品A和B的厚度、波长、亮度对比表Table 1 Comparison table of thickness, wavelength and brightness of epitaxial wafer samples A and B
图4是采用本申请方法制备外延片样品A并使用PL(光致发光测试仪)测试样品GaN基材料厚度的分布图以及采用对比实施例的工艺制备外延片样品B使用PL(光致发光测试仪)测试样品GaN基材料厚度的分布图。从图4可明显看出,采用本申请方法制备的样片A的GaN基材料厚度分布在6.85μm-6.93μm,片内厚度差值为0.08μm,具有很好的均匀性。而采用对比实施例工艺制备的样品B的GaN材料厚度分布在6.88μm-7.07μm,片内厚度差值为0.19μm,均匀性较差。Fig. 4 is a distribution diagram of the thickness of epitaxial wafer sample A prepared by the method of the present application and tested using PL (photoluminescence tester) and the thickness of the GaN-based material of the sample and the process of using the comparative example to prepare epitaxial wafer sample B using PL (photoluminescence tester) Instrument) The distribution diagram of the thickness of the test sample GaN-based material. It can be clearly seen from Fig. 4 that the thickness of the GaN-based material of sample A prepared by the method of the present application is distributed between 6.85 μm and 6.93 μm, and the thickness difference within the chip is 0.08 μm, which has good uniformity. However, the thickness of the GaN material of the sample B prepared by the process of the comparative example is distributed between 6.88 μm and 7.07 μm, and the thickness difference within the chip is 0.19 μm, and the uniformity is poor.
上述样品A的厚度均匀性得到明显改善的原因是:本申请方法中加入的应力释放层具有比高温GaN更好的松弛度,能很好释放GaN与AlN模板直接的晶格应力,改善了外延生长时wafer的翘曲,使片内温度变得更加均匀,即提高了外延生长时片内长速的一致性,因此提高了GaN材料的厚度均匀性。The reason why the thickness uniformity of the above-mentioned sample A has been significantly improved is that the stress release layer added in the method of this application has better relaxation than high-temperature GaN, which can well release the direct lattice stress between GaN and AlN templates, and improves the epitaxy. The warping of the wafer during growth makes the temperature in the chip more uniform, which improves the consistency of the growth rate in the chip during epitaxial growth, thus improving the thickness uniformity of the GaN material.
图5是采用本申请方法制备外延片样品A并使用PL(光致发光测试仪)测试样品A波长的分布图以及采用对比实施例的工艺制备外延片样品B使用PL(光致发光测试仪)测试样品B波长的分布图。从图5可看出,样品A的波长分布在455.87nm-457.33nm,差值为1.46nm,具有很好的片内均匀性,而样品B的波长分布在440.6-467.42nm,差值为26.86nm,均匀性很差,对外延片制作成芯片后的帅选工作造成很大困扰。Fig. 5 is the distribution diagram of the wavelength of sample A prepared by the method of the present application and tested by PL (photoluminescence tester) and the sample B of epitaxial wafer prepared by the process of comparative example by using PL (photoluminescence tester) Distribution plot of test sample B wavelength. It can be seen from Figure 5 that the wavelength distribution of sample A is 455.87nm-457.33nm, with a difference of 1.46nm, which has good intra-chip uniformity, while the wavelength distribution of sample B is 440.6-467.42nm, with a difference of 26.86nm nm, the uniformity is very poor, causing a lot of trouble for the handsome selection work after the epitaxial wafer is made into a chip.
上述样品A的波长均匀性得到明显改善的原因是:加入的应力释放层很好的释放了GaN材料因晶格失配带来的应力,是wafer在生长量子阱时的片内温度变均匀,因而得到较高的波长一致性。The reason why the wavelength uniformity of the above-mentioned sample A has been significantly improved is that the stress release layer added can well release the stress caused by the lattice mismatch of the GaN material, which is why the temperature inside the wafer becomes uniform when growing quantum wells. Thus a higher wavelength uniformity is obtained.
图6是采用本申请方法制备外延片样品A并使用PL(光致发光测试仪)测试样品A发光强度的分布图以及采用对比实施例的工艺制备外延片样品B使用PL(光致发光测试仪)测试样品B发光强度的分布图。从图6可看出,样品A的发光强度分布在19.9-21.76,差值为1.86,均匀性很好,而样品B的发光强度分布在8.87-20.34,差值为11.47,均匀性很差。Fig. 6 is a distribution diagram of the luminous intensity of the sample A prepared by the method of the present application and tested using the PL (photoluminescence tester) sample A and the process of the comparative example to prepare the epitaxial wafer sample B using the PL (photoluminescence tester) ) The distribution diagram of the luminous intensity of test sample B. It can be seen from Figure 6 that the luminous intensity distribution of sample A is 19.9-21.76, the difference is 1.86, and the uniformity is very good, while the luminous intensity of sample B is distributed between 8.87-20.34, the difference is 11.47, and the uniformity is very poor.
上述样品A具有较高发光强度均匀性的原因是:加入应力释放层后,wafer表面温度变得均匀,使外延在生长每个结构时的一致性都得到提高,发光强度自然也具有更好的均匀性;另外,波长的均匀性的提高表明样品A的量子阱区域InGaN分布更均匀,有利于提高外延片的亮度及其均匀性。The reason why the above-mentioned sample A has higher uniformity of luminous intensity is that after adding the stress release layer, the surface temperature of the wafer becomes uniform, which improves the consistency of the epitaxial growth of each structure, and the luminous intensity naturally has better Uniformity; In addition, the increase in the uniformity of the wavelength indicates that the distribution of InGaN in the quantum well region of sample A is more uniform, which is beneficial to improving the brightness and uniformity of the epitaxial wafer.
综上,本申请所提供的改善LED芯片性能均匀性的外延生长方法,通过引入应力释放层,能明显弱化晶格失配和热失配带来的负面效应,改善了外延片片内波长、厚度、亮度的均匀性,有利于溅射AlN生长GaN外延技术的广泛推广。In summary, the epitaxial growth method for improving the performance uniformity of LED chips provided by this application can significantly weaken the negative effects caused by lattice mismatch and thermal mismatch by introducing a stress release layer, and improve the wavelength, The uniformity of thickness and brightness is conducive to the widespread promotion of sputtering AlN growth GaN epitaxial technology.
通过以上各实施例可知,本申请存在的有益效果是:Can know by above each embodiment, the beneficial effect that the present application exists is:
(1)本发明改善LED芯片性能均匀性的外延生长方法,与传统方法相比,加入了应力释放层,该应力释放层具有比高温GaN更好的松弛度,能很好释放GaN与AlN模板直接的晶格应力,改善了外延生长时wafer的翘曲,使片内温度变得更加均匀,即提高了外延生长时片内长速的一致性,因此提高了GaN材料的厚度均匀性。(1) The epitaxial growth method of the present invention to improve the performance uniformity of the LED chip, compared with the traditional method, adds a stress release layer, the stress release layer has better relaxation than high-temperature GaN, and can release GaN and AlN templates well The direct lattice stress improves the warpage of the wafer during epitaxial growth and makes the temperature inside the chip more uniform, that is, improves the consistency of the growth rate in the chip during epitaxial growth, thus improving the thickness uniformity of GaN materials.
(2)本发明改善LED芯片性能均匀性的外延生长方法,加入的应力释放层很好的释放了GaN材料因晶格失配带来的应力,使wafer在生长量子阱时的片内温度变均匀,因而得到较高的波长一致性。(2) The epitaxial growth method of the present invention improves the performance uniformity of the LED chip, and the added stress release layer well releases the stress caused by the lattice mismatch of the GaN material, so that the internal temperature of the wafer when growing the quantum well changes. Uniform, thus obtaining higher wavelength consistency.
(3)本发明改善LED芯片性能均匀性的外延生长方法,加入应力释放层后,wafer表面温度变得均匀,使外延在生长每个结构时的一致性都得到提高,发光强度自然也具有更好的均匀性;另外,波长的均匀性的提高表明样品A的量子阱区域InGaN分布更均匀,有利于提高外延片的亮度及其均匀性。(3) The epitaxial growth method of the present invention improves the performance uniformity of the LED chip. After adding the stress release layer, the surface temperature of the wafer becomes uniform, so that the consistency of the epitaxial growth of each structure is improved, and the luminous intensity is naturally higher. Good uniformity; in addition, the increase in the uniformity of the wavelength indicates that the distribution of InGaN in the quantum well region of sample A is more uniform, which is conducive to improving the brightness and uniformity of the epitaxial wafer.
本领域内的技术人员应明白,本申请的实施例可提供为方法、装置、或计算机程序产品。因此,本申请可采用完全硬件实施例、完全软件实施例、或结合软件和硬件方面的实施例的形式。而且,本申请可采用在一个或多个其中包含有计算机可用程序代码的计算机可用存储介质(包括但不限于磁盘存储器、CD-ROM、光学存储器等)上实施的计算机程序产品的形式。Those skilled in the art should understand that the embodiments of the present application may be provided as methods, apparatuses, or computer program products. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment, or an embodiment combining software and hardware aspects. Furthermore, the present application may take the form of a computer program product embodied on one or more computer-usable storage media (including but not limited to disk storage, CD-ROM, optical storage, etc.) having computer-usable program code embodied therein.
上述说明示出并描述了本申请的若干优选实施例,但如前所述,应当理解本申请并非局限于本文所披露的形式,不应看作是对其他实施例的排除,而可用于各种其他组合、修改和环境,并能够在本文所述发明构想范围内,通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本申请的精神和范围,则都应在本申请所附权利要求的保护范围内。The above description shows and describes several preferred embodiments of the present application, but as mentioned above, it should be understood that the present application is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various Various other combinations, modifications, and environments can be made within the scope of the inventive concept described herein, by the above teachings or by skill or knowledge in the relevant field. However, modifications and changes made by those skilled in the art do not depart from the spirit and scope of the present application, and should all be within the protection scope of the appended claims of the present application.
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