CN1313655C - Method for growing high-mobility gallium nitride epitaxial film - Google Patents
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Abstract
一种生长高迁移率氮化镓外延膜的方法,其特征在于,包括如下步骤:先在衬底上采用金属有机物化学气相沉积生长一层低温氮化镓成核层;随后升高衬底的温度,在低温氮化镓成核层上生长氮化镓恢复层;最后在生长室压力为400-600torr条件下,在氮化镓恢复层上生长非有意掺杂氮化镓层,室温迁移率不小于400cm2/V.s。
A method for growing a high-mobility GaN epitaxial film, characterized in that it comprises the following steps: first growing a layer of low-temperature GaN nucleation layer on a substrate by metal-organic chemical vapor deposition; Temperature, grow a gallium nitride recovery layer on the low-temperature gallium nitride nucleation layer; finally, grow a non-intentionally doped gallium nitride layer on the gallium nitride recovery layer under the condition of a growth chamber pressure of 400-600torr, and the room temperature mobility Not less than 400cm 2 /Vs.
Description
技术领域technical field
本发明属于半导体技术领域,特别指室温迁移率不小于400cm2/V.s的氮化镓外延膜的外延生长方法。The invention belongs to the technical field of semiconductors, in particular to an epitaxial growth method of a gallium nitride epitaxial film with room temperature mobility not less than 400 cm 2 /Vs.
背景技术Background technique
III-V族氮化镓材料作为第三代半导体材料的典型代表,由于具有独特的物理、化学和机械性能,在光电子和微电子领域有着巨大的应用前景。氮化镓材料可用于制备HEMT、HFET、HBT、JFET、MOSFET、SAW等器件。迁移率是表征材料质量的重要参数,高迁移率材料的获得对材料研究和器件研制具有很大的益处。但是由于缺少与氮化镓材料相匹配的异质衬底材料,材料的纯度难以提高,因此难以获得高迁移率的GaN材料。As a typical representative of the third-generation semiconductor materials, III-V gallium nitride materials have great application prospects in the fields of optoelectronics and microelectronics due to their unique physical, chemical and mechanical properties. GaN materials can be used to prepare HEMT, HFET, HBT, JFET, MOSFET, SAW and other devices. Mobility is an important parameter to characterize the quality of materials, and the acquisition of high mobility materials is of great benefit to material research and device development. However, due to the lack of heterogeneous substrate materials that match GaN materials, the purity of the materials is difficult to improve, so it is difficult to obtain GaN materials with high mobility.
在本发明以前,经常采用的高迁移率氮化镓材料的生长方法是:先在衬底蓝宝石(0001)或其它适于生长氮化物的衬底的晶面上采用金属有机物化学气相沉积(MOCVD)生长一层低温氮化镓成核层,然后升高衬底温度,生长不掺杂或者Si掺杂的氮化镓层以提高迁移率。如果使用掺杂的方法,掺杂的原子虽然能提高GaN材料的迁移率,但是掺杂的原子破坏了GaN原本的晶格,导致GaN材料的晶体质量下降。因此这种方法会影响材料本身和由其制备的器件性能。对于非掺杂直接生长本征GaN的方法,目前迁移率大多在200~500cm2/V.s范围。因此如何进一步提高非掺杂的GaN材料的迁移率,是氮化物材料发展的一个重要问题。Before the present invention, the growth method of the high-mobility gallium nitride material that often adopts is: adopt metal-organic chemical vapor deposition (MOCVD) on the crystal plane of substrate sapphire (0001) or other substrates suitable for growing nitrides ) to grow a low-temperature GaN nucleation layer, and then increase the substrate temperature to grow an undoped or Si-doped GaN layer to improve mobility. If the doping method is used, although the doped atoms can improve the mobility of the GaN material, the doped atoms destroy the original crystal lattice of GaN, resulting in a decrease in the crystal quality of the GaN material. This approach therefore affects the performance of the material itself and the devices fabricated from it. For the method of directly growing intrinsic GaN without doping, the current mobility is mostly in the range of 200-500 cm 2 /Vs. Therefore, how to further improve the mobility of non-doped GaN materials is an important issue in the development of nitride materials.
发明内容Contents of the invention
本发明的目的在于提供一种生长高迁移率氮化镓外延膜的方法,其方法是通过非有意掺杂,通过控制生长条件,如温度、压力以及加入氮化镓恢复层的新结构,有效缓解了晶格失配带来的应力,提高了晶体质量。生长出了高迁移率的本征氮化镓材料。本发明还提高了样品表面的平整度。The purpose of the present invention is to provide a method for growing high-mobility gallium nitride epitaxial film, which method is through non-intentional doping, by controlling the growth conditions, such as temperature, pressure and adding a new structure of gallium nitride recovery layer, effectively The stress caused by lattice mismatch is relieved and the crystal quality is improved. A high-mobility intrinsic GaN material is grown. The invention also improves the flatness of the sample surface.
本发明一种生长高迁移率氮化镓外延膜的方法,其特征在于,包括如下步骤:The present invention is a method for growing a high-mobility GaN epitaxial film, which is characterized in that it comprises the following steps:
先在衬底上采用金属有机物化学气相沉积生长一层低温氮化镓成核层;First grow a low-temperature gallium nitride nucleation layer on the substrate by metal-organic chemical vapor deposition;
随后升高衬底的温度,在低温氮化镓成核层上生长氮化镓恢复层;Then increase the temperature of the substrate, and grow a gallium nitride recovery layer on the low-temperature gallium nitride nucleation layer;
最后在生长室压力为400-600torr条件下,在氮化镓恢复层上生长非有意掺杂氮化镓层,室温迁移率不小于400cm2/V.s。Finally, under the condition that the growth chamber pressure is 400-600 torr, a non-intentionally doped gallium nitride layer is grown on the gallium nitride recovery layer, and the mobility at room temperature is not less than 400cm 2 /Vs.
其中所述的衬底为蓝宝石或硅或碳化硅或GaLiO3、ZnO。The substrate mentioned therein is sapphire or silicon or silicon carbide or GaLiO 3 , ZnO.
其中在衬底上生长低温氮化镓成核层时,衬底的温度为500-600℃,压力为400-600torr,生长厚度为0.01-0.06μm。When growing the low-temperature GaN nucleation layer on the substrate, the temperature of the substrate is 500-600° C., the pressure is 400-600 torr, and the growth thickness is 0.01-0.06 μm.
其中氮化镓恢复层的生长温度1000-1100℃之间,生长压力100-300torr,生长厚度为0.1-0.3μm。Wherein, the growth temperature of the gallium nitride recovery layer is between 1000-1100° C., the growth pressure is 100-300 torr, and the growth thickness is 0.1-0.3 μm.
其中非有意掺杂高迁移率氮化镓层生长温度为1000-1100℃之间,氮化镓膜厚为0.5-6μm。The growth temperature of the non-intentionally doped high-mobility gallium nitride layer is between 1000-1100° C., and the thickness of the gallium nitride film is 0.5-6 μm.
附图说明Description of drawings
为进一步说明本发明的内容,以下结合具体实施方式对本发明作一详细的描述,其中:To further illustrate the contents of the present invention, the present invention will be described in detail below in conjunction with specific embodiments, wherein:
图1是本发明的本征高迁移率GaN层生长结构示意图;1 is a schematic diagram of the growth structure of the intrinsic high mobility GaN layer of the present invention;
图2是本发明的高迁移率GaN材料的迁移率及载流子浓度随温度的变化曲线;Fig. 2 is the variation curve of the mobility and carrier concentration of the high mobility GaN material of the present invention with temperature;
图3是本发明的高迁移率GaN X射线摇摆曲线半峰宽测试结果;Fig. 3 is high mobility GaN X-ray rocking curve half peak width test result of the present invention;
图4是本发明的高迁移率GaN表面粗糙度RMS测试结果。Fig. 4 is the RMS test result of the surface roughness of the high mobility GaN of the present invention.
具体实施方式Detailed ways
本发明关键在于加入氮化镓恢复层的新结构和生长了非有意掺杂的高迁移率氮化镓外延膜。通过控制生长条件,如温度、压力到最佳的条件,配合加入的氮化镓恢复层新结构,最大限度的消除了晶格与衬底失配带来的应力,而应力正是产生晶体位错的主要原因。另一方面,非有意掺杂的氮化镓外延层有效降低了由于掺杂而引起的电离杂质,从而提高了晶体质量,生长出了高迁移率的本征氮化镓材料。本发明还提高了样品表面的平整度。The key of the invention lies in adding a new structure of gallium nitride recovery layer and growing non-intentionally doped high-mobility gallium nitride epitaxial film. By controlling the growth conditions, such as temperature and pressure to the optimum conditions, and with the addition of the new structure of the GaN recovery layer, the stress caused by the mismatch between the crystal lattice and the substrate is eliminated to the greatest extent, and the stress is the one that generates the crystal position. The main reason for the error. On the other hand, the non-intentionally doped GaN epitaxial layer effectively reduces the ionized impurities caused by doping, thereby improving the crystal quality and growing an intrinsic GaN material with high mobility. The invention also improves the flatness of the sample surface.
请参阅图1所示,本发明一种生长高迁移率氮化镓外延膜的方法,包括如下步骤:Please refer to Fig. 1, a method for growing a high-mobility gallium nitride epitaxial film of the present invention, comprising the following steps:
先在衬底10上采用金属有机物化学气相沉积(MOCVD)生长一层低温氮化镓成核层20;其中所述的衬底10为蓝宝石或硅或碳化硅或GaLiO3、ZnO;其中在衬底10上生长低温氮化镓成核层20时,衬底10的温度为500-600℃,压力为400-600torr,生长厚度为0.01-0.06μm;First grow a layer of low-temperature gallium nitride nucleation layer 20 on the substrate 10 by metal-organic chemical vapor deposition (MOCVD); wherein the substrate 10 is sapphire or silicon or silicon carbide or GaLiO 3 , ZnO; wherein the substrate When growing the low-temperature gallium nitride nucleation layer 20 on the substrate 10, the temperature of the substrate 10 is 500-600° C., the pressure is 400-600 torr, and the growth thickness is 0.01-0.06 μm;
随后升高衬底10的温度,在低温氮化镓成核层20上生长氮化镓恢复层30;其中氮化镓恢复层30的生长温度1000-1100℃之间,生长压力100-300torr,生长厚度为0.1-0.3μm;Then increase the temperature of the substrate 10, and grow the gallium nitride recovery layer 30 on the low-temperature gallium nitride nucleation layer 20; wherein the growth temperature of the gallium nitride recovery layer 30 is between 1000-1100° C., and the growth pressure is 100-300 torr, The growth thickness is 0.1-0.3μm;
最后改变生长室压力,在氮化镓恢复层30上生长非有意掺杂高迁移率氮化镓层40;其中非有意掺杂高迁移率氮化镓层40生长温度为1000-1100℃之间,生长压力为400-600torr,氮化镓膜厚为0.5-6μm。Finally, change the pressure of the growth chamber to grow the non-intentionally doped high-mobility GaN layer 40 on the GaN recovery layer 30; wherein the growth temperature of the non-intentionally doped high-mobility GaN layer 40 is between 1000-1100°C , the growth pressure is 400-600torr, and the gallium nitride film thickness is 0.5-6μm.
用此方法生长的氮化镓为高迁移率氮化镓,室温迁移率不小于400cm2/V.s。The gallium nitride grown by this method is high-mobility gallium nitride, and the mobility at room temperature is not less than 400 cm 2 /Vs.
实施例Example
结合参阅图1,本发明一种生长高迁移率氮化镓外延膜的方法,包括如下步骤:Referring to Fig. 1, a method for growing a high-mobility gallium nitride epitaxial film of the present invention comprises the following steps:
1、在衬底10蓝宝石(0001)或硅(111)或碳化硅(0001)或其它适于生长氮化物的衬底如GaLiO3、ZnO等的晶面上采用金属有机物化学气相沉积(MOCVD)生长一层低温氮化镓成核层。衬底温度约500-600℃,压力为400-600torr,生长厚度0.01-0.06μm。1. Metal-organic chemical vapor deposition (MOCVD) is used on the substrate 10 sapphire (0001) or silicon (111) or silicon carbide (0001) or other substrates suitable for growing nitrides, such as GaLiO 3 , ZnO, etc. A low-temperature gallium nitride nucleation layer is grown. The substrate temperature is about 500-600° C., the pressure is 400-600 torr, and the growth thickness is 0.01-0.06 μm.
2、之后升高衬底10温度,生长氮化镓恢复层,氮化镓恢复层的生长温度1000-1100℃之间,生长压力100-300torr,生长厚度为0.1-0.3μm。2. Afterwards, the temperature of the substrate 10 is increased to grow the gallium nitride recovery layer. The growth temperature of the gallium nitride recovery layer is between 1000-1100° C., the growth pressure is 100-300 torr, and the growth thickness is 0.1-0.3 μm.
3、最后改变生长室压力,非有意掺杂高迁移率氮化镓层,生长温度在1000-1100℃之间,生长压力为400-600torr,氮化镓膜厚约0.5-6μm。3. Finally, change the growth chamber pressure, unintentionally dope the high-mobility gallium nitride layer, the growth temperature is between 1000-1100°C, the growth pressure is 400-600torr, and the thickness of the gallium nitride film is about 0.5-6μm.
对由以上步骤获得的样品进行测试分析,证明用此方法生长的氮化镓为高迁移率氮化镓材料。使用范德堡HALL测试方法证实在室温300K时该材料迁移率大于730cm2/V.s,载流子浓度1.8×1016cm-3,77K时迁移率1580cm2/V.s,载流子浓度4.0×1015cm-3(图2);同时晶体质量得到了改善,使用双晶X射线衍射方法证实该材料的(0002)面的摇摆曲线半峰宽小于6arcmin.(图3);原子力显微镜(AFM)测试方法证实该材料表面粗糙度(RMS)为0.159nm(图4)。本发明降低了工艺难度,减少了工艺步骤,一次性地生长出了高质量的本征高迁移率氮化镓材料,优化了生长工艺。The samples obtained by the above steps are tested and analyzed, and it is proved that the gallium nitride grown by this method is a high-mobility gallium nitride material. Using the Vanderbilt HALL test method, it was confirmed that the mobility of the material is greater than 730cm 2 /Vs at room temperature 300K, the carrier concentration is 1.8×10 16 cm -3 , and the mobility at 77K is 1580cm 2 /Vs, and the carrier concentration is 4.0×10 15 cm -3 (Figure 2); at the same time, the crystal quality has been improved, and the half-maximum width of the rocking curve of the (0002) plane of the material is confirmed to be less than 6arcmin. (Figure 3) using a twin-crystal X-ray diffraction method; atomic force microscopy (AFM) The test method confirmed that the material had a surface roughness (RMS) of 0.159nm (Figure 4). The invention reduces the difficulty of the process, reduces the steps of the process, grows the high-quality intrinsically high-mobility gallium nitride material at one time, and optimizes the growth process.
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| CN100395379C (en) * | 2005-12-15 | 2008-06-18 | 南京大学 | A method for growing highly crystalline indium nitride single crystal epitaxial film |
| CN100549243C (en) * | 2006-07-05 | 2009-10-14 | 武汉华灿光电有限公司 | A method for epitaxial growth of AlxGa1-xN single crystal thin film on sapphire substrate material |
| CN101519799B (en) * | 2008-02-27 | 2012-11-21 | 中国科学院半导体研究所 | Method for preparing non-polar GaN thick film on sapphire substrate |
| CN101812725B (en) * | 2010-04-09 | 2011-08-31 | 中国科学院半导体研究所 | Growth method of phase-change nucleation in epitaxy of gallium nitride |
| CN115548102A (en) * | 2022-06-28 | 2022-12-30 | 徐州金沙江半导体有限公司 | Growth method of gallium nitride HEMT epitaxial structure |
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| CN1365136A (en) * | 2001-01-12 | 2002-08-21 | 中国科学院半导体研究所 | Method for producing III family nitride single/multiple layer heterogeneous strain film |
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| Characteristics of AlGaN/GaN HEM Ts Grown byPlasma-Assisted Molecular Beam Epitaxy Wang Xiaoliang et al,半导体学报,第25卷第2期 2004 * |
| NH3-MBE生长极化场二维电子气材料 孙殿照等,功能材料与器件学报,第6卷第4期 2000 * |
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