高质量单晶金刚石的合成、结构与光学性能研究

屠菊萍; 刘金龙; 邵思武; 朱肖华; 赵云; 陈良贤; 魏俊俊; 李成明

doi:doi:10.3788/AOS202040.0631001

光学学报, 2020, 40 (6): 0631001, 网络出版: 2020-03-06

高质量单晶金刚石的合成、结构与光学性能研究下载： 1868次

Synthesis, Structure, and Optical Properties of a High-Quality Single-Crystal Diamond

论文大纲

屠菊萍刘金龙 ^*邵思武朱肖华赵云陈良贤魏俊俊李成明

作者单位

北京科技大学新材料技术研究院, 北京 100083

薄膜高质量单晶金刚石透过率光学吸收系数痕量杂质 thin film high-quality single-crystal diamond transmittance optical absorption coefficient trace impurities

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摘要

采用微波等离子体化学气相沉积法通过控制痕量杂质制备了高质量单晶金刚石材料,并对其结构与光学性能进行综合评价。通过紫外可见吸收光谱和光致发光谱分析了晶体的杂质及含量;采用拉曼光谱、摇摆曲线及X射线白光形貌束分析了不同质量单晶体的晶体结构及结晶质量;通过偏光显微镜综合评价了不同质量单晶金刚石的晶体结构和缺陷。结果证明:获得的高纯单晶金刚石含有少量的缺陷、杂质,其位错应力场以聚集状均匀分布,高纯单晶金刚石与微掺氮单晶金刚石在紫外可见近红外波段的透过率最高可分别达到71.58%和71.27%,接近单晶金刚石的理论透过率(71.6%),且在本征红外吸收波段,高纯金刚石晶体相对微掺氮单晶金刚石,对称性较好,样品吸光度较小。控制痕量杂质制备的高质量单晶金刚石膜有望应用于光探测器探头和光学窗口。

Abstract

In this study, microwave plasma chemical vapor deposition was used to control the trace impurities for preparing high-quality single-crystal diamond materials, the structural and optical properties of which were comprehensively evaluated. Further, the impurity contents of the crystals were analyzed using ultraviolet (UV)-visible absorption spectroscopy and photoluminescence spectra. The crystal structures and quality of the single crystals exhibiting different qualities were analyzed based on the Raman spectrum, X-ray rocking curve, and X-ray white-light morphology beam. Subsequently, the crystal structures and defects of a single-crystal diamond exhibiting different qualities were evaluated under a polarizing microscope. The obtained high-purity single-crystal diamond contains a few defects and impurities, and its dislocation stress field is uniformly distributed in the aggregate state. The maximum transmittances of single-crystal diamonds with high purity and low-doped nitrogen in the UV visible near-infrared (UV-visible-NIR) band are 71.58% and 71.27%, respectively, which are approximately similar to the theoretical value of transmittance (71.6%) for diamond. In the intrinsic infrared absorption band, the lattice symmetry of high-purity diamond crystals is better, whereas the absorbance is smaller than that of low-concentration nitrogen-doped single-crystal diamonds. The high-quality single-crystal diamond film prepared by controlling the trace impurities is expected to be used as an optical detector probe and an optical window.

1 引言

金刚石作为功能材料,具有优异的光学性质,除在3~6 μm双声子波段具有本征吸收峰外,几乎是全波段透明的,在光学领域有着重要的应用前景^[1-2]。金刚石是一种重要的辐射探测材料^[3],在高能物理辐射探测方面已占据无可替代的位置^[4]。化学气相沉积(chemical vapor deposition,CVD) 金刚石探测技术可以作为 X光二极管探测技术的良好补充^[5]。高质量 CVD 金刚石膜的研制为金刚石辐射探测器的研发开辟了新的路径^[6]。此外,在众多的红外光学窗口材料中,金刚石兼具众多优异性能,因而受到了人们的广泛关注^[7]。目前国外采用微波等离子体化学气相沉积(MPCVD)法制备的高质量金刚石膜,已作为窗口材料应用于工业领域。如金刚石膜在真空电子器件中使用时,可克服散热及高功率毫米波和回旋管器件输能窗中的问题^[8]。

金刚石的光学性质及结晶质量与制备过程中的杂质种类及含量有密切关系^[9]。制备高纯单晶金刚石以及比较不同杂质含量金刚石的光学性能对于金刚石在光学领域的拓展应用具有重要意义。氮原子是金刚石中一种最普遍的杂质,可与碳原子形成多种复合形式,直接影响金刚石的光学性质,进而限制金刚石的光学用途^[10]。氮主要通过共价键与其他原子结合,由于氮的原子半径与碳的原子半径很接近,因此氮原子容易进入金刚石晶体中并占据其晶格位置形成杂质原子,由于氮原子比碳原子多一个电子,氮原子多余的电子在金刚石中形成色心而使金刚石晶体呈现出多种颜色, 从而导致金刚石物理性质发生改变^[11]。此外CVD过程中,氮的存在不仅可以促进单晶金刚石的台阶生长,稳定单晶金刚石的外延生长模式,还可以提升金刚石的生长速率。除此之外,在CVD制备过程中会通入适量的氧气,这是因为低浓度的O₂可促进沉积并改善晶体质量^[12-13]。

本文通过控制痕量杂质制备了不同质量等级的高质量单晶金刚石材料,研究了金刚石材料内杂质、结构缺陷与光学性质,综合分析了材料内杂质、结构缺陷对光学性能的影响规律。

2 实验方法

本实验中高质量单晶金刚石样品均使用课题组自主设计的 6 kW,2.45 GHz新型穹顶式微波装置完成。籽晶分别经丙酮和酒精超声波清洗后,放入真空度低于0.1 Pa的微波化学气相沉积腔室中。生长前使用H₂/O₂等离子体刻蚀1 h,去除表面的化学吸附杂质,消除由于机械加工导致的表面损伤层。之后通过控制氧气与氮气原子数分数分别生长高纯单晶金刚石与微掺氮单晶金刚石,高纯样品采用的衬底是抛光的(100)面的高温高压籽晶,薄膜生长并抛光后的厚度为0.20 mm,微掺氮样品是以高纯CVD样品为籽晶,薄膜生长并抛光后得到的厚度为0.44 mm,两种样品的具体沉积参数如表1所示。其中,氢气体积分数为99.9999%,甲烷、氮气和氧气体积分数均为99.999%。此外,还采用日本市售的厚度为0.54 mm的单晶金刚石晶片作为参照样品进行对比分析。

表 1. 高纯与微掺氮单晶金刚石沉积工艺参数表

Table 1. Deposition parameters of single crystal diamonds with high purity and low-doped nitrogen

Deposition parameter	High-purity single crystal diamond	Low-concentration nitrogen doped single crystal diamond
Flow of etching gas $\begin{matrix} {H_{2}}_{} \end{matrix}$ /sccm	300	300
Flow of etching gas $\begin{matrix} {O_{2}}_{} \end{matrix}$ /sccm	3	3
Etching temperature /℃	700±10	700±10
Etching time /h	1	1
Deposition temperature /℃	750±5	780±5
Flow of CH₄, H₂, N₂, $\begin{matrix} {O_{2}}_{} \end{matrix}$ /sccm	15, 300, 0, 1.2	15, 300, 0.9, 0

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采用inVia-Reflex型显微拉曼谱仪对晶体中的金刚石相和非晶碳相进行拉曼表征和光致发光(PL)表征,以分析金刚石中杂质及缺陷信息,测试温度均为室温,激发波长为532 nm,采用1800 lp/mm的光栅。采用Varian Cary 7000 型紫外可见近红外(UV-visible-NIR)分光光度计表征样品的透过率和吸光度。采用Excalibur 3100型傅里叶变换红外光谱仪表征样品的红外(IR)透过率。采用XPert-MRD型 X射线衍射装置进行摇摆曲线测试,扫描步长为 0.0002°,扫描电压为40 kV,电流为30 mA。X射线使用Cu的K_α1光线,单色器为 Ge(220)四晶单色器,探测器为正比计数器,仪器本征半峰全宽(HWHM)为12″。采用X射线白光形貌技术观察金刚石中的位错分布状态,样品与胶片的距离为5.5 cm,所用胶片来自Fuji Kogyo,型号为Fuji IX-50,储环运行参数为2.5 GeV、250 mA,样品与光源的距离为42 m。

3 结果与讨论

3.1 高纯与微掺氮单晶金刚石杂质分析

CVD金刚石中掺杂的氮主要以替位式氮原子存在,单晶中氮杂质的原子数分数可以通过替位氮原子在270 nm处的吸收峰进行计算^[14-15],即N=0.56×ΔA^[15],其中N为金刚石中孤氮原子数分数,ΔA为在270 nm处,测得的光谱曲线与拟合曲线纵坐标之间的差值。图1所示实线为高纯、微掺氮单晶金刚石和参照样品的紫外吸收光谱,虚线为对300~450 nm处的光谱进行三阶多项式拟合并反向延长得到的曲线,发现只有参照样品在270 nm处含有孤氮的特征峰,高纯单晶金刚石样品没有孤氮的特征峰,微掺氮单晶金刚石样品含有非常微弱的孤氮特征峰。根据上述公式进一步计算可以得到高纯、微掺氮单晶金刚石和参照样品中的孤氮原子数分数分别为:3.73×10^-9、4.99×10^-9、6.887×10^-8。除此之外,采用二次离子质谱(SIMS)测试了高纯样品的氮浓度,其结果低于探测器的检测极限10^-7。

图 1. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的紫外可见吸收光谱。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 1. UV-visible absorption spectra of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

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除去替位氮之外,CVD金刚石单晶中常见的氮杂质类型还有^[16]:中性[N-V]⁰和负电[N-V]^-,他们分别对应光致发光谱中的波长575 nm和637 nm,如图2所示,而695 nm附近的宽峰与[N-V]色心有关^[17]。当晶体中存在大量缺陷、杂质时,光致发光(PL)会非常明显^[18]。由样品的PL图可知,参照样品和微掺氮金刚石都存在氮杂质,但是参照样品中含有更多的[N-V]⁰和[N-V]^-,且其荧光背底强度也较高。高纯单晶金刚石的PL谱线中不含氮的相关峰位,只有一个很强的金刚石峰,而且其背底相比于另外其他两个样品强度较平坦,这表明通过不掺氮并结合少量氧原子可以有效抑制金刚石中痕量氮原子的原子数分数,进而得到十分纯净的金刚石晶体。高纯单晶金刚石晶体中杂质密度较低是因为活性氧原子可以通过去除或减少等离子体中N和Si相关杂质来净化外延层^[19]。

图 2. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的PL图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 2. PL diagram of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

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3.2 高纯与微掺氮单晶金刚石的晶体结构宏观表征

采用正交偏光显微镜能够观察单晶金刚石表面或内部的状态和对应力敏感的缺陷。金刚石单晶属于立方晶系,为均质体,故理论上在正交偏振光下会完全消光,但是在单晶内部由于结构受应力的影响,会引起光性反常现象。图3为采用正交偏光显微镜在透射光模式下得到的图像,其中高亮部分为杂质或者位错比较集中的区域,可以观察到高纯单晶金刚石内部存在少量应力分布,微掺氮单晶金刚石位错较多但分布均匀,而在参照样品中具有十分明显的应力集中区,由高的位错密度等缺陷构成。相比于参照样品,高纯样品和微掺氮样品质量较高。

图 3. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的正交偏光显微图(透射光)。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 3. Cross polarized micrograph (transmitted light) of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

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图4给出样品的拉曼图,可知三个样品在1332 cm^-1附近都具有很窄的金刚石特征峰,参照样品在1442.5 cm^-1处具有含氮的荧光峰,这是由于N的存在,金刚石晶体中出现了局部能级,当样品受到紫外线照射时,样品晶体结构中的原子外层电子发生跃迁,释放能量,产生荧光^[20],且在1600 cm^-1后谱线向上漂移,这说明该单晶金刚石膜的拉曼谱中出现了背底,这是由金刚石膜的光致发光引起的^[21-23]。高纯单晶金刚石在1332.1 cm^-1处只有一个金刚石特征峰,无杂峰存在,这说明该样品为高质量单晶金刚石。微掺氮单晶金刚石为掺入体积分数约0.3%的氮气得到的单晶金刚石,由拉曼峰可知,除了较强的金刚石特征峰,还存在含氮的荧光峰,但相比于参照样品来说,荧光峰较弱,该样品含有更少的氮。

图 4. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的拉曼光谱图

Fig. 4. Raman spectra of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

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对于理想晶体,严格按照空间点阵排列,其半峰全宽应该为零,但实际上晶体在结晶时晶格和取向不完全一致,存在一定的展宽,宽度越大说明晶体取向较差,所以在一定程度上,半峰全宽反映了结晶的好坏^[24]。拉曼峰的半峰全宽表征了样品的结晶质量,如果晶体内存在缺陷等晶格畸变,那么晶体拉曼谱的半峰全宽将会变宽^[25,26]。天然完美金刚石半峰全宽低至1.5 cm^-1,CVD生长的单晶金刚石膜半峰全宽可低至1.6~1.8 cm^-1[27]。由三者的拉曼谱线对其采用洛伦兹拟合,得到如图5所示的高纯、微掺氮单晶金刚石和参照样品的拟合曲线,可以得到其半峰全宽分别为:w_p=2.03 cm^-1,w_d=4.10 cm^-1,w_r=4.46 cm^-1。杂质和晶体内部缺陷均会引起单晶金刚石拉曼特征峰半峰全宽的宽化,高纯单晶金刚石半峰全宽更接近天然完美金刚石半峰全宽,说明生长过程中等离子体中氧原子的存在可提高晶体质量。

3.3 高纯与微掺氮单晶金刚石的晶体缺陷评价

采用X射线摇摆曲线评估单晶金刚石的结晶质量及位错状态。对于单晶金刚石而言,一般通过研究其(400)晶面的 X 射线衍射峰的摇摆曲线来表征其结晶质量和位错密度。X 射线摇摆曲线的半峰全宽越低,表明其晶体的结晶质量越好^[28]。对于单晶金刚石来说,由于只有单一的摇摆曲线衍射峰,无法使用线性拟合,因此晶体位错密度可表示为^[29-31]

\begin{matrix} ρ = β_{h kl}^{2} / (9 b^{2}), \end{matrix}

式中:β_hkl为半峰全宽,hkl为晶面指数,这里指(400)晶面;b为晶体位错的柏氏矢量。图6为高纯、微掺氮单晶金刚石膜和参照样品的(400)晶面的摇摆曲线图,由三者的半峰全宽数值可以计算得到位错密度分别为:ρ_p=3.928×10⁶ cm^-2,ρ_d=8.907×10⁶ cm^-2,ρ_r=1.014×10⁷ cm^-2,图中横坐标表示该晶面与样品面的夹角,其范围从-θ至+θ。这从很大程度上反映了晶体内部的缺陷状态,由于高纯金刚石采用的是高质量高温高压衬底,因此得到的摇摆曲线半峰全宽最小,位错密度最小,微掺氮单晶金刚石采用的是CVD衬底,且掺入了氮杂质,其半峰全宽较大,参照样品摇摆曲线的半峰全宽最大。

图 5. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品拟合后的Raman光谱图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 5. Fitted Raman spectra of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

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图 6. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的摇摆曲线。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 6. X-ray rocking curve of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

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X射线白光形貌是一种分析晶体材料微观结构缺陷的方法,可以显示晶体的缺陷及其分布状况^[32]。图7分别为参照样品、高纯、微掺氮单晶金刚石的X射线白光形貌图像,显示了晶体的缺陷及其分布情况,图中g表征衍射面。图中较暗的区域的衍射强度较高,这与畸变区域和晶格缺陷有关。位错的产生与籽晶表面的预处理及生长过程中的等离子体的状态有关,若籽晶中存在较多位错,会导致生长过程中从界面处引入更多位错,进而在后续直接生长过程中使位错遗传生长。当在生长过程中掺入少量的氧气,氢氧等离子体因其具有各向异性刻蚀的特点,会在位错处优先刻蚀,可减少外延层的位错。

高纯、微掺氮单晶金刚石白光形貌图如图7(a)和图7(b)所示,图中较暗的区域都是由位错产生的应力场,但二者应力场的分布不同,高纯单晶金刚石内部位错纠缠成结,应力场以聚集状均匀分布,而微掺氮单晶金刚石的应力场呈线性分布,应力场面积占据整个晶体。参照样品的白光形貌图如图7(c)所示,图中整个晶体都呈现暗的状态,原因在于:等离子体中含有较多氮杂质,增加了晶体的晶格参数,形成张应力,增加了位错成核的概率;晶体整体扩展位错较多。

图 7. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的X射线白光形貌图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 7. X-ray white light topography of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

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3.4 高质量单晶金刚石的光学性质

红外光谱检测的是分子的振动和转动能量^[33]。图8给出三者的吸光度图,由图可知,三者的红外吸收峰均在1332~2664 cm^-1之间,这是金刚石C—C晶格振动产生的本征双声子吸收峰。CVD金刚石在生长过程中引入了杂质和空隙等缺陷,导致晶格点阵的对称性遭到破坏,从而产生了红外活性,引起红外吸收^[34]。由图8可知,在本征吸收波段,高纯单晶金刚石吸光度远低于微掺氮及参照样品的吸光度,微掺氮金刚石的吸光度略低于参照样品的吸光度,这说明氮杂质的存在破坏了样品的晶格点阵,使样品吸光度增加。

图 8. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的红外吸光度图

Fig. 8. Infrared absorbance diagram of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

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图9所示为三个样品的紫外可见红外(UV-visible-IR)透过率,图中虚线左边为通过紫外可见近红外分光光度计得到的谱线,右边是采用傅里叶变换红外光谱仪得到的曲线。在紫外可见近红外波段,高纯和微掺氮透过率最大分别达到了71.58%和71.27%,接近相应波段金刚石的理论透过率(71.60%),参照样品透过率略低,最高值为69.86%。在中红外波段,其中双声子区域存在本征吸收,透过率显著降低,且化学气相沉积金刚石膜在生长过程中会引入N、H及sp²-C等杂质,杂质越多透过率越差。除双声子区域外的红外波段,光子与晶格发生作用并不能产生偶极矩,没有红外活性^[35],三者透过率均较高。

图 9. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的UV-visible-IR透过率

Fig. 9. UV-visible-IR transmittance of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

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4 结论

采用微波化学气相沉积法通过控制痕量杂质制备了高质量单晶金刚石材料。通过紫外可见吸收光谱和PL谱得到高纯金刚石中孤氮原子数分数仅为3.73×10^-9。N原子的存在使微掺氮金刚石在1442.5 cm^-1附近具有含氮的荧光峰,而高纯单晶金刚石仅在1332.1 cm^-1处存在明显的金刚石特征峰,无杂峰存在。通过(400)晶面的 X 射线衍射峰的摇摆曲线得到了高纯、微掺氮单晶金刚石的位错密度分别为:3.928×10⁶ cm^-2、8.907×10⁶ cm^-2。白光形貌图和正交偏光显微图直观显示了高纯单晶金刚石内部存在纠缠成结以聚集状均匀分布的位错应力场,而微掺氮金刚石中存在更多位错应力场,应力敏感区域更大。在紫外可见近红外波段,高纯、微掺氮单晶金刚石具有接近金刚石此波段理论值的透过率。高纯样品在本征红外吸收波段具有较小的吸光度,其晶格点阵的对称性较好。由于控制痕量杂质制备的单晶金刚石质量高,光学性能极佳,故有望用于光探测器探头和光学窗口。

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3.2 高纯与微掺氮单晶金刚石的晶体结构宏观表征

3.3 高纯与微掺氮单晶金刚石的晶体缺陷评价

3.4 高质量单晶金刚石的光学性质

4 结论

屠菊萍, 刘金龙, 邵思武, 朱肖华, 赵云, 陈良贤, 魏俊俊, 李成明. 高质量单晶金刚石的合成、结构与光学性能研究[J]. 光学学报, 2020, 40(6): 0631001. Juping Tu, Jinlong Liu, Siwu Shao, Xiaohua Zhu, Yun Zhao, Liangxian Chen, Junjun Wei, Chengming Li. Synthesis, Structure, and Optical Properties of a High-Quality Single-Crystal Diamond[J]. Acta Optica Sinica, 2020, 40(6): 0631001.

高质量单晶金刚石的合成、结构与光学性能研究下载： 1868次

1 引言

2 实验方法

表 1. 高纯与微掺氮单晶金刚石沉积工艺参数表

Table 1. Deposition parameters of single crystal diamonds with high purity and low-doped nitrogen

3 结果与讨论

3.1 高纯与微掺氮单晶金刚石杂质分析

图 1. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的紫外可见吸收光谱。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 1. UV-visible absorption spectra of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 2. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的PL图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 2. PL diagram of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

3.2 高纯与微掺氮单晶金刚石的晶体结构宏观表征

图 3. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的正交偏光显微图(透射光)。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 3. Cross polarized micrograph (transmitted light) of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 4. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的拉曼光谱图

Fig. 4. Raman spectra of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

3.3 高纯与微掺氮单晶金刚石的晶体缺陷评价

图 5. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品拟合后的Raman光谱图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 5. Fitted Raman spectra of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 6. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的摇摆曲线。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 6. X-ray rocking curve of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 7. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的X射线白光形貌图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 7. X-ray white light topography of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

3.4 高质量单晶金刚石的光学性质

图 8. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的红外吸光度图

Fig. 8. Infrared absorbance diagram of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

图 9. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的UV-visible-IR透过率

Fig. 9. UV-visible-IR transmittance of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

4 结论

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高质量单晶金刚石的合成、结构与光学性能研究 下载： 1868次

1 引言

2 实验方法

表 1. 高纯与微掺氮单晶金刚石沉积工艺参数表

Table 1. Deposition parameters of single crystal diamonds with high purity and low-doped nitrogen

3 结果与讨论

3.1 高纯与微掺氮单晶金刚石杂质分析

图 1. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的紫外可见吸收光谱。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 1. UV-visible absorption spectra of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 2. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的PL图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 2. PL diagram of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

3.2 高纯与微掺氮单晶金刚石的晶体结构宏观表征

图 3. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的正交偏光显微图(透射光)。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 3. Cross polarized micrograph (transmitted light) of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 4. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的拉曼光谱图

Fig. 4. Raman spectra of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

3.3 高纯与微掺氮单晶金刚石的晶体缺陷评价

图 5. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品拟合后的Raman光谱图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 5. Fitted Raman spectra of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 6. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的摇摆曲线。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 6. X-ray rocking curve of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

图 7. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的X射线白光形貌图。(a)高纯单晶金刚石;(b)微掺氮单晶金刚石;(c)参照样品

Fig. 7. X-ray white light topography of three kinds of single crystal diamonds. (a) Single crystal diamond with high purity; (b) single crystal diamond with low-doped nitrogen; (c) reference sample

3.4 高质量单晶金刚石的光学性质

图 8. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的红外吸光度图

Fig. 8. Infrared absorbance diagram of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

图 9. 高纯单晶金刚石、微掺氮单晶金刚石和参照样品的UV-visible-IR透过率

Fig. 9. UV-visible-IR transmittance of single crystal diamond with high purity, single crystal diamond with low-doped nitrogen and reference sample

4 结论

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高质量单晶金刚石的合成、结构与光学性能研究下载： 1868次