CVD金刚石单晶生长及金刚石晶体管的研究
摘要
金刚石兼具多方面优异性质，是最重要的半导体材料之一，在众多领域具有十分重要的应用价值。近年来，高品质化学气相沉积（CVD）金刚石单晶的生长及高性能金刚石半导体器件的研究，成为金刚石领域前沿和热点研究课题。
高品质CVD金刚石的获得依赖于生长条件的控制和优化。另外，金刚石在制备大功率电子器件方面具有独特的优势，而其栅极材料的选用十分重要。目前，用作金刚石晶体管的常用栅极氧化物为Al_2O_3，SiO_2，CaF_2等，然而这些材料的介电常数较低，无法实现对金刚石高空穴密度的完全控制，其他具有较高介电常数的绝缘材料（如铁电材料）往往需要引入合适的过渡层。因此，选择一种新型的栅极绝缘材料，是实现高性能大功率金刚石晶体管器件的关键。
本论文采用微波等离子体CVD（MPCVD）方法，研究了生长过程中反应气氛对CVD金刚石单晶的生长速率和质量的影响。在金刚石衬底上利用不同方法进行了氧化钽（Ta_2O_5）和氧化铪（HfO_2）的沉积，研究了氧化物及金刚石/氧化物异质结的电学性质，并以Ta_2O_5为栅极材料制作了金刚石晶体管原型器件。主要成果如下：
一、CVD金刚石单晶的生长。
1、传统高速生长CVD金刚石单晶的气氛条件（H_2/CH_4/N_2=500sccm/60sccm/1.8sccm）下，分别通入不同流量二氧化碳（CO_2）气体，生长金刚石单晶。金刚石的生长速率随着CO_2流量的增加，呈现出先上升、后下降的趋势。引入CO2所制备的同质外延CVD金刚石单晶的结晶质量较好。
2、采用温室气体笑气（N_2O）来辅助生长金刚石单晶。N_2O中的氮氧共同作用，可以在提高CVD金刚石质量的同时，提高了生长速率。引入最佳流量的N_2O气体（H_2/CH_4/N_2O=750sccm/90sccm/2sccm），CVD金刚石单晶生长速率最大，并且质量最好。
3、在金刚石相关器件研究中，金刚石层厚度、表面形貌及质量的控制十分重要。我们研究了在氢气（H_2，500sccm）中不同甲烷（CH_4，1060sccm）流量下CVD金刚石单晶的生长。较低CH_4流量条件下，金刚石单晶生长速率较低，表面光滑平整，利于金刚石半导体器件的制作。随着CH_4流量的增加，生长速率提高，和碳源的增加有密切的关系，但此时样品表面出现非外延生长晶粒，不利于制作半导体器件。
二、高介电常数（k）氧化物栅极金刚石晶体管的研究
1、提出以Ta_2O_5作为金刚石晶体管的栅极材料，利用射频溅射法直接在金刚石上沉积得到非晶态Ta_2O_5薄膜，经氮气气氛中经800oC快速退火，获得六角相-Ta_2O_5。非晶态Ta_2O_5具有良好的绝缘体性质，其相对介电常数为16，C-V特性中表现出明显的迟滞现象。退火可以提高薄膜介电常数，达到29，消除C-V曲线中的迟滞现象，但是增大了MOS结构的漏电流。
经过对导电机制及束缚电荷密度的分析，我们认为退火作用提高了晶体质量，因此消除了C-V特性中的迟滞现象，但是在Ta_2O_5/金刚石界面附近引入了束缚电荷使得漏电流增加。
以Ta_2O_5为栅极绝缘材料制备了金刚石晶体管原型器件，器件表现出明显的栅极电压对漏极电流的显著控制作用。
2、利用原子层沉积法和射频溅射法，在金刚石衬底上制备出较高品质的HfO_2薄膜，介电常数约为20，C-V曲线中的迟滞效应与制备方法有关，该工作为研制以HfO_2薄膜为栅极氧化物的金刚石晶体管奠定了一定的基础。
本文系统地研究了CVD金刚石单晶的生长及金刚石晶体管原型器件的制备和电学特性，得到了有价值的结果，为开发新一代高性能金刚石基半导体器件打下一定的研究基础。
Diamond is a new functional material with many excellent properties, which hasbeen widely applied in many fields. Recently, the chemical vapor deposition (CVD)high quality single crystal diamonds (SCDs) and high performance diamond-basedsemiconductor devices have become hot topic issues in diamond researches. Thegrowth of high quality SCDs is dependent on the deposition conditions. Moreover,the selected suitable gate material plays an important role in improving theperformance of diamond-based high-power electronic devices.
In this thesis, we systemically investigate the growth of SCDs under variousreaction ambient. For the diamond field-effect transistor (FET), the deposition,structure, and electronic properties of the high dielectric constant (k) materials oftantalum pentoxide (Ta_2O_5) and hafnium dioxide (HfO_2) thin films on SCD substratesare studied. Using Ta_2O_5as gate material, the prototype diamond FETs wereconstructed, which are favorable for realizing a new generation of high-performancediamond-based devices. The main content and innovation of this thesis are listed asfollowing:
(1) The gaseous carbon dioxide (CO_2) was introduced into the traditionalreaction feeding gases of H_2/CH_4/N_2=500/60/1.8in sccm to examine the growthbehaviors of the SCDs with adding CO_2. The growth rate increases at lower flowrates of CO_2, and then decreases with a larger amount, which can be attributed to thecompetition between the increasing carbon source and enhanced oxygen etchinginduced by CO_2. The homoepitaxial SCDs layers show good crystalline quality.
(2) The greenhouse gas nitrous oxide (N_2O) was introduced into the H_2/CH_4ambient to assist the growth of CVD SCDs. The combination of the N-and O-relatedradicals generating from N2O are favorable for not only improving the quality ofSCDs, but also increasing the growth rate. The optimized growth condition is of H_2/CH_4/N_2O=750/90/2in sccm to realize high quality and high-rate growth ofhomoepitaxial SCDs.
(3) The growth of CVD diamond crystals has been investigated at different CH4flow rates (10,20,40,60sccm) in H_2(500sccm) plasma at a constant reactionpressure of200torr. The growth rates of SCDs are increased from2to15m/h withincreasing the flow rates of CH4. The surface of the high quality SCDs grown at lowCH4flow rates are smooth. However, at higher CH4flow rates, there are someunepitaxial grains appearing on the growth surface of the SCDs, which are notconducive to further fabricate high performance diamond-based devices.
(4) The Ta_2O_5has been proposed as the gate material for diamond transistor.Synthesized by radio frequency sputtering, the as deposited Ta_2O_5films on p-typediamond substrate were amorphous having good insulating behavior and a dielectricconstant (k) of16. The corresponding C-V characteristic shows an obvious hysteresisphenomenon. After rapid thermal annealing in a nitrogen atmosphere at800oC, ahexagonal-Ta_2O_5film was obtained and the k value was markedly improved to be29. In this case, the hysteresis phenomenon of the C-V curve was eliminated,meanwhile, the leakage current of the MOS structure was increased. These variationscan be attributed to the annealing-induced quality improvement of Ta_2O_5film andincrease of trapped charge near the interface of Ta_2O_5/diamond. Experimentally, theprototype diamond FET with Ta_2O_5as the gate material shows obvious control ofdrain current by the gate voltage.
(5) By the methods of atomic layer deposition and radio frequency sputtering,higher quality HfO_2films with a high K of~20have been deposited on diamondsubstrate. It is found that the hysteresis effect in the corresponding C-V curves of therelated MOS structures is strongly dependent on the deposition method.
高品质CVD金刚石的获得依赖于生长条件的控制和优化。另外，金刚石在制备大功率电子器件方面具有独特的优势，而其栅极材料的选用十分重要。目前，用作金刚石晶体管的常用栅极氧化物为Al_2O_3，SiO_2，CaF_2等，然而这些材料的介电常数较低，无法实现对金刚石高空穴密度的完全控制，其他具有较高介电常数的绝缘材料（如铁电材料）往往需要引入合适的过渡层。因此，选择一种新型的栅极绝缘材料，是实现高性能大功率金刚石晶体管器件的关键。
本论文采用微波等离子体CVD（MPCVD）方法，研究了生长过程中反应气氛对CVD金刚石单晶的生长速率和质量的影响。在金刚石衬底上利用不同方法进行了氧化钽（Ta_2O_5）和氧化铪（HfO_2）的沉积，研究了氧化物及金刚石/氧化物异质结的电学性质，并以Ta_2O_5为栅极材料制作了金刚石晶体管原型器件。主要成果如下：
一、CVD金刚石单晶的生长。
1、传统高速生长CVD金刚石单晶的气氛条件（H_2/CH_4/N_2=500sccm/60sccm/1.8sccm）下，分别通入不同流量二氧化碳（CO_2）气体，生长金刚石单晶。金刚石的生长速率随着CO_2流量的增加，呈现出先上升、后下降的趋势。引入CO2所制备的同质外延CVD金刚石单晶的结晶质量较好。
2、采用温室气体笑气（N_2O）来辅助生长金刚石单晶。N_2O中的氮氧共同作用，可以在提高CVD金刚石质量的同时，提高了生长速率。引入最佳流量的N_2O气体（H_2/CH_4/N_2O=750sccm/90sccm/2sccm），CVD金刚石单晶生长速率最大，并且质量最好。
3、在金刚石相关器件研究中，金刚石层厚度、表面形貌及质量的控制十分重要。我们研究了在氢气（H_2，500sccm）中不同甲烷（CH_4，1060sccm）流量下CVD金刚石单晶的生长。较低CH_4流量条件下，金刚石单晶生长速率较低，表面光滑平整，利于金刚石半导体器件的制作。随着CH_4流量的增加，生长速率提高，和碳源的增加有密切的关系，但此时样品表面出现非外延生长晶粒，不利于制作半导体器件。
二、高介电常数（k）氧化物栅极金刚石晶体管的研究
1、提出以Ta_2O_5作为金刚石晶体管的栅极材料，利用射频溅射法直接在金刚石上沉积得到非晶态Ta_2O_5薄膜，经氮气气氛中经800oC快速退火，获得六角相-Ta_2O_5。非晶态Ta_2O_5具有良好的绝缘体性质，其相对介电常数为16，C-V特性中表现出明显的迟滞现象。退火可以提高薄膜介电常数，达到29，消除C-V曲线中的迟滞现象，但是增大了MOS结构的漏电流。
经过对导电机制及束缚电荷密度的分析，我们认为退火作用提高了晶体质量，因此消除了C-V特性中的迟滞现象，但是在Ta_2O_5/金刚石界面附近引入了束缚电荷使得漏电流增加。
以Ta_2O_5为栅极绝缘材料制备了金刚石晶体管原型器件，器件表现出明显的栅极电压对漏极电流的显著控制作用。
2、利用原子层沉积法和射频溅射法，在金刚石衬底上制备出较高品质的HfO_2薄膜，介电常数约为20，C-V曲线中的迟滞效应与制备方法有关，该工作为研制以HfO_2薄膜为栅极氧化物的金刚石晶体管奠定了一定的基础。
本文系统地研究了CVD金刚石单晶的生长及金刚石晶体管原型器件的制备和电学特性，得到了有价值的结果，为开发新一代高性能金刚石基半导体器件打下一定的研究基础。
Diamond is a new functional material with many excellent properties, which hasbeen widely applied in many fields. Recently, the chemical vapor deposition (CVD)high quality single crystal diamonds (SCDs) and high performance diamond-basedsemiconductor devices have become hot topic issues in diamond researches. Thegrowth of high quality SCDs is dependent on the deposition conditions. Moreover,the selected suitable gate material plays an important role in improving theperformance of diamond-based high-power electronic devices.
In this thesis, we systemically investigate the growth of SCDs under variousreaction ambient. For the diamond field-effect transistor (FET), the deposition,structure, and electronic properties of the high dielectric constant (k) materials oftantalum pentoxide (Ta_2O_5) and hafnium dioxide (HfO_2) thin films on SCD substratesare studied. Using Ta_2O_5as gate material, the prototype diamond FETs wereconstructed, which are favorable for realizing a new generation of high-performancediamond-based devices. The main content and innovation of this thesis are listed asfollowing:
(1) The gaseous carbon dioxide (CO_2) was introduced into the traditionalreaction feeding gases of H_2/CH_4/N_2=500/60/1.8in sccm to examine the growthbehaviors of the SCDs with adding CO_2. The growth rate increases at lower flowrates of CO_2, and then decreases with a larger amount, which can be attributed to thecompetition between the increasing carbon source and enhanced oxygen etchinginduced by CO_2. The homoepitaxial SCDs layers show good crystalline quality.
(2) The greenhouse gas nitrous oxide (N_2O) was introduced into the H_2/CH_4ambient to assist the growth of CVD SCDs. The combination of the N-and O-relatedradicals generating from N2O are favorable for not only improving the quality ofSCDs, but also increasing the growth rate. The optimized growth condition is of H_2/CH_4/N_2O=750/90/2in sccm to realize high quality and high-rate growth ofhomoepitaxial SCDs.
(3) The growth of CVD diamond crystals has been investigated at different CH4flow rates (10,20,40,60sccm) in H_2(500sccm) plasma at a constant reactionpressure of200torr. The growth rates of SCDs are increased from2to15m/h withincreasing the flow rates of CH4. The surface of the high quality SCDs grown at lowCH4flow rates are smooth. However, at higher CH4flow rates, there are someunepitaxial grains appearing on the growth surface of the SCDs, which are notconducive to further fabricate high performance diamond-based devices.
(4) The Ta_2O_5has been proposed as the gate material for diamond transistor.Synthesized by radio frequency sputtering, the as deposited Ta_2O_5films on p-typediamond substrate were amorphous having good insulating behavior and a dielectricconstant (k) of16. The corresponding C-V characteristic shows an obvious hysteresisphenomenon. After rapid thermal annealing in a nitrogen atmosphere at800oC, ahexagonal-Ta_2O_5film was obtained and the k value was markedly improved to be29. In this case, the hysteresis phenomenon of the C-V curve was eliminated,meanwhile, the leakage current of the MOS structure was increased. These variationscan be attributed to the annealing-induced quality improvement of Ta_2O_5film andincrease of trapped charge near the interface of Ta_2O_5/diamond. Experimentally, theprototype diamond FET with Ta_2O_5as the gate material shows obvious control ofdrain current by the gate voltage.
(5) By the methods of atomic layer deposition and radio frequency sputtering,higher quality HfO_2films with a high K of~20have been deposited on diamondsubstrate. It is found that the hysteresis effect in the corresponding C-V curves of therelated MOS structures is strongly dependent on the deposition method.
引文
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