CN103205729A - 用ald设备生长氮化镓薄膜的方法 - Google Patents
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- 238000000231 atomic layer deposition Methods 0.000 title claims abstract description 24
- 229910002601 GaN Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 17
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 46
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 29
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 6
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 claims description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 6
- 238000010306 acid treatment Methods 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- 239000012159 carrier gas Substances 0.000 claims description 2
- 238000006557 surface reaction Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 2
- 230000000802 nitrating effect Effects 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002140 halogenating effect Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
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- 230000005693 optoelectronics Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
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Abstract
本发明公开用ALD设备生长氮化镓薄膜的方法,包括步骤10、将碳化硅衬通过标准液和氢氟酸处理处理表面并放置于原子层沉积设备反应腔中;步骤20、向所述原子层沉积设备反应腔中通入镓源气体,所述镓源气体作为第一反应前驱体源在碳化硅衬底表面进行化学吸附,所述镓源气体中的镓原子吸附在所述碳化硅衬底上;步骤30、吸附在碳化硅衬底上的镓原子与电离后的第二反应前驱体在氢气的辅助下发生反应,直到所述碳化硅衬底表面的镓原子完全消耗;重复步骤20、30,即可在所述碳化硅衬底表面形成氮化镓薄膜。本发明提供的方法能够实现均匀的在整个结构中掺氮,且掺杂后氮元素含量高,薄膜结构完整。
Description
技术领域
本发明涉及氮化镓材料的制备,具体涉及一种用ALD设备生长氮化镓薄膜的方法。
背景技术
GaN材料的研究与应用是目前半导体研究的前沿和热点,是研制微电子器件、光电子器件的新型半导体材料,是LED产业发展的基础。GaN材料具有宽的直接带隙,高的热导率和击穿电场,介电常数小,抗辐射能力强,且化学稳定性好(几乎不被任何酸腐蚀),在光电子、高温大功率器件和高频微波器件应用方面有着广阔的前景。在LED产业中,具有完整结构的GaN材料及具有匹配的晶体常数直接影响到LED的性能。
目前,GaN的外延生长工艺一般有以下几种:MOCVD,MBE,LEO和PECVD等。MOCVD是制备GaN及其相关多层结构薄膜的主流技术,具有价格较低、生长速度快等特点。但是其生长温度过高,一般高于900℃,这容易造成制备出的GaN薄膜少氮和存在碳污染。在低温条件下,使用等离子体辅助的方式是一种较好的办法,但是通过PECVD方法制作出的结果并不理想。
发明内容
本发明所要解决的技术问题是提供一种能够实现对GaN薄膜的生长,且生长出的GaN薄膜含有较高的氮含量,且制备方法简单,掺杂后的薄膜结构完整,氮含量提升,性能显著增加的用ALD设备生长氮化镓薄膜的方法。
为解决上述技术问题,本发明提供了一种用ALD设备生长氮化镓薄膜的方法,包括:
步骤10、将碳化硅衬通过标准液和氢氟酸处理处理表面并放置于原子层沉积设备反应腔中;
步骤20、向所述原子层沉积设备反应腔中通入镓源气体,所述镓源气体作为第一反应前驱体源在碳化硅衬底表面进行化学吸附,所述镓源气体中的镓原子吸附在所述碳化硅衬底上;
步骤30、吸附在碳化硅衬底上的镓原子与电离后的第二反应前驱体在氢气的辅助下发生反应,直到所述碳化硅衬底表面的镓原子完全消耗;
重复步骤20、30,即可在所述碳化衬底表面形成氮化镓薄膜。
进一步地,所述镓源气体是氯化镓;所述氯化镓通过和衬底表面反应而进行化学吸附。
进一步地,所述电离后的第二前驱体是载气氮气,所述氮气电离后的氮气分子与氢气形成氮氢离子,和氯化镓中的氯原子发生反应,使得氯化镓中除镓以外的其他官能团被氮原子取代。
进一步地,在所述步骤20和步骤30之前分别包括向原子层沉积设备反应腔通入清洗气体清洗腔室。
进一步地,所述清洗气体为氮气。
本发明提供的用ALD设备生长氮化镓薄膜的方法,操作简单,转化率高,能耗小,利用原子层沉积单层循环生长的特点,能够实现均匀的在整个结构中掺氮,且掺杂后氮元素含量高,薄膜结构完整。
附图说明
图1为本发明实施例中碳化硅表面形成Si-H键的示意图;
图2为本发明实施例中氯化镓和碳化硅衬底表面发生卤代反应,镓原子吸附在碳化硅衬底上的示意图;
图3为本发明实施例中碳化硅衬底表面被镓原子吸附后的示意图;
图4为本发明实施例中向原子层沉积反应腔通入氢气,并进行氮气等离子体放电电离的示意图;
图5为本发明实施例中氮气电离后,碳化硅衬底表面形成具有氢原子的镓氮结构的示意图。
具体实施方式
参见图1,本发明实施例提供的一种用ALD设备生长氮化镓薄膜的方法包括:
步骤101、通过标准液和氢氟酸处理碳化硅衬底表面,在碳化硅衬底表面形成硅氢键,如图1所示,其中,标准液是指:1号液,浓硫酸∶双氧水=4∶1;2号液,氨水∶纯净水∶双氧水=1∶5∶1;3号液,盐酸∶双氧水∶纯净水=1∶1∶6;将进行氢化处理后的碳化硅衬底放置于原子层沉积设备反应腔中;
步骤102、开启原子层沉积设备,调整工作参数,达到实验所需工作环境;先向原子层沉积设备反应腔通入氮气清洗腔室,然后向原子层沉积反应腔中通入镓源气体,如图2所示;氮化镓和碳化硅衬底表面的氢原子发生反应,镓原子吸附在碳化硅衬底表面,如图3所示;
步骤103、先向原子层沉积设备反应腔通入氮气清洗腔室,然后向原子层沉积设备反应腔中通入氢气,氢气的速率为2sccm-10sccm,并进行氮气等离子放电,等离子体放电功率为1W-100W,氮气电离后的氮气分子与氢气形成氮氢离子,和氯化镓中的氯原子发生反应(如图4所示),使得氯化镓中除镓以外的其他官能团被氮原子取代,碳化硅衬底表面形成具有氢原子的镓氮结构(如图5所示)。
步骤104,步骤102至步骤103这一反应周期结束后,碳化硅衬底表面全为氢原子,此时重复步骤102至步骤103,可以逐层生长氮化镓薄膜。
本发明提供的用ALD设备生长氮化镓薄膜的方法,操作简单,转化率高,能耗小,利用原子层沉积单层循环生长的特点,能够实现均匀的在整个结构中掺氮,且掺杂后氮元素含量高,薄膜结构完整。
最后所应说明的是,以上具体实施方式仅用以说明本发明的技术方案而非限制,尽管参照实例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (5)
1.一种用ALD设备生长氮化镓薄膜的方法,其特征在于,包括:
步骤10、将碳化硅衬通过标准液和氢氟酸处理处理表面并放置于原子层沉积设备反应腔中;
步骤20、向所述原子层沉积设备反应腔中通入镓源气体,所述镓源气体作为第一反应前驱体源在碳化硅衬底表面进行化学吸附,所述镓源气体中的镓原子吸附在所述碳化硅衬底上;
步骤30、吸附在碳化硅衬底上的镓原子与电离后的第二反应前驱体在氢气的辅助下发生反应,直到所述碳化硅衬底表面的镓原子完全消耗;
重复步骤20、30,即可在所述碳化衬底表面形成氮化镓薄膜。
2.根据权利要求1所述的方法,其特征在于:
所述镓源气体是氯化镓;所述氯化镓通过和衬底表面反应而进行化学吸附。
3.根据权利要求1所述的方法,其特征在于:
所述电离后的第二前驱体是载气氮气,所述氮气电离后的氮气分子与氢气形成氮氢离子,和氯化镓中的氯原子发生反应,使得氯化镓中除镓以外的其他官能团被氮原子取代。
4.根据权利要求1所述的方法,其特征在于,在所述步骤20和步骤30之前分别包括:
向原子层沉积设备反应腔通入清洗气体清洗腔室。
5.根据权利要求1所述的方法,其特征在于:
所述清洗气体为氮气。
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CN106449907A (zh) * | 2016-11-18 | 2017-02-22 | 电子科技大学 | 一种p型指数掺杂结构GaN光电阴极材料的生长方法 |
CN106449907B (zh) * | 2016-11-18 | 2019-04-12 | 电子科技大学 | 一种p型指数掺杂结构GaN光电阴极材料的生长方法 |
CN112221524A (zh) * | 2020-09-16 | 2021-01-15 | 西安近代化学研究所 | 一种负载型大比表面积氮化镓催化剂的制备方法 |
CN112221524B (zh) * | 2020-09-16 | 2023-01-13 | 西安近代化学研究所 | 一种负载型大比表面积氮化镓催化剂的制备方法 |
CN112985330A (zh) * | 2021-02-07 | 2021-06-18 | 西安交通大学 | 一种用于在线仪器校准的晶圆级膜厚标准片的制备方法 |
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