热管理用3英寸硅衬底金刚石薄膜的制备

doi:10.15541/jim20230476

无机材料学报 ›› 2024, Vol. 39 ›› Issue (3): 283-290.DOI: 10.15541/jim20230476 CSTR: 32189.14.10.15541/jim20230476

所属专题：【信息功能】大尺寸功能晶体(202409)

热管理用3英寸硅衬底金刚石薄膜的制备

杨志亮¹(), 杨鏊¹, 刘鹏¹, 陈良贤¹, 安康², 魏俊俊¹, 刘金龙¹, 吴立枢³(), 李成明¹()

1.北京科技大学新材料技术研究院, 北京 100083
2.北方工业大学机械与材料工程学院, 北京 100144
3.中国电子科技集团公司第五十五研究所, 固态微波器件与电路全国重点实验室, 南京 210016

收稿日期:2023-10-16 修回日期:2023-11-12 出版日期:2024-03-20 网络出版日期:2023-12-04
通讯作者: 吴立枢, 高级工程师. E-mail: wulishu117@163.com;
李成明, 教授. E-mail: chengmli@master.ustb.edu.cn
作者简介:杨志亮(1994-), 男, 博士研究生. E-mail: 1220715584@qq.com
基金资助:
固态微波器件与电路全国重点实验室基金;国家自然科学基金(52172037);国家自然科学基金(52102034);北方工业大学有组织科研(2023YZZKY12)

Preparation of 3-inch Diamond Film on Silicon Substrate for Thermal Management

YANG Zhiliang¹(), YANG Ao¹, LIU Peng¹, CHEN Liangxian¹, AN Kang², WEI Junjun¹, LIU Jinlong¹, WU Lishu³(), LI Chengming¹()

1. Institute for Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083, China
2. School of Mechanical and Materials Engineering, North China University of Technology, Beijing 100114, China
3. National Key Laboratory of Solid-State Microwave Devices and Circuits, The 55th Research Institute of China Electronics Technology Group Corporation, Nanjing 210016, China

Received:2023-10-16 Revised:2023-11-12 Published:2024-03-20 Online:2023-12-04
Contact: WU Lishu, senior engineer. E-mail: wulishu117@163.com;
LI Chengming, professor. E-mail: chengmli@master.ustb.edu.cn
About author:YANG Zhiliang (1994-), male, PhD candidate. E-mail: 1220715584@qq.com
Supported by:
National Key Laboratory of Solid-State Microwave Devices and Circuits;National Natural Science Foundation of China(52172037);National Natural Science Foundation of China(52102034);Organized Research Fund of North China University of Technology(2023YZZKY12)

摘要/Abstract

摘要：

金刚石膜材料用作GaN电子器件散热器具有巨大潜力, 低应力、大尺寸、高质量、原子级光滑表面的金刚石膜层是GaN器件的整体传热能力提升的关键。本研究提出了一种用于3英寸(1英寸=2.54 cm)硅衬底多晶金刚石薄膜的生长和晶圆级抛光技术, 用以实现大尺寸金刚石膜材料在散热器方向上的应用。首先对微波谐振腔内的等离子体进行多物理场自洽建模, 通过仿真模拟技术分析2.45 GHz多模椭球谐振腔微波等离子体化学气相沉积(Microwave plasma chemical vapor deposition, MPCVD)装置沉积大尺寸金刚石薄膜的可行性, 并优化生长工艺参数。然后对金刚石薄膜进行研磨抛光处理, 以满足GaN器件的键合需求。模拟结果表明, 输入相同的微波功率, 腔室压强增大导致等离子核心电子和原子H数密度增加, 但径向分布均匀性变差。在优化的工艺条件下沉积了金刚薄膜。实验结果表明, 金刚石薄膜厚度不均匀性为17%。较高的甲烷浓度导致金刚石晶粒呈现以(111)晶面为主的金字塔形貌特征, 并伴有孪晶的生成。Raman光谱中金刚石一阶特征峰半峰全宽(Full width at half maximum, FWHM)为7.4 cm⁻¹。抛光后表面粗糙度达到0.27 nm, 硅衬底金刚石薄膜平均弯曲度为13.84 μm, 平均内应力为−40.7 MPa。采用上述方法, 成功制备了大尺寸、较高晶体质量、低内应力、原子级光滑表面的硅衬底金刚石晶圆。

关键词: 金刚石薄膜, MPCVD, 晶圆级抛光

Abstract:

The diamond film material holds great potential as a heat sink for GaN electronic devices. The diamond film layer with low stress, large dimensions, high quality, and an atomically smooth surface is crucial for enhancing the overall heat transfer capacity of GaN devices. This study presents a technique for growing and polishing polycrystalline diamond films on 3-inch(1 inch=2.54 cm) silicon substrates to facilitate the use of large-sized diamond film materials in radiator applications. Firstly, the study carries out multi-physical field self-consistent modelling of plasma in a microwave resonator. It then analyses the feasibility of depositing large diamond films using a microwave plasma chemical vapour deposition (MPCVD) device with a 2.45 GHz multi-mode ellipsoid resonator through simulation technology. The growth process parameters are optimized accordingly. After that, the diamond film is polished to meet the bonding requirements of GaN devices. The simulation results show that under the same microwave power input, the increase of chamber pressure leads to the increase of number density of plasma core electrons and H atoms, but the uniformity of radial distribution becomes worse. Diamond film is deposited under optimized conditions and mensurates that the thickness inhomogeneity of diamond film is 17%. In this process, methane at high concentration leads to pyramidal morphology of diamond grains dominated by (111) planes, accompanied by formation of twins. Full width at half maximum (FWHM) of the first-order characteristic peak of diamond in Raman spectrum is 7.4 cm⁻¹. After polishing, the surface roughness reaches 0.27 nm, the average bending degree of diamond film on silicon substrate is 13.84 μm, and the average internal stress is −40.7 MPa. Silicon substrate diamond wafers with large size, high crystal quality, low internal stress and atomically smooth surface are successfully prepared by the above method.

Key words: diamond film, MPCVD, wafer level polishing

中图分类号:

O484

杨志亮, 杨鏊, 刘鹏, 陈良贤, 安康, 魏俊俊, 刘金龙, 吴立枢, 李成明. 热管理用3英寸硅衬底金刚石薄膜的制备[J]. 无机材料学报, 2024, 39(3): 283-290.

YANG Zhiliang, YANG Ao, LIU Peng, CHEN Liangxian, AN Kang, WEI Junjun, LIU Jinlong, WU Lishu, LI Chengming. Preparation of 3-inch Diamond Film on Silicon Substrate for Thermal Management[J]. Journal of Inorganic Materials, 2024, 39(3): 283-290.

图/表 9

图1 MPCVD装置中微波电场的三维谐振模式图

Fig. 1 Three-dimensional resonance mode diagram of microwave electric field in MPCVD device

表1 碰撞反应的集合[21]

Table 1 Set of collision reactions [21]

Num.	Electron collision reaction	Collision type	Energy loss/eV
1	$e+{{\text{H}}_{2}}\to e+{{\text{H}}_{2}}$	Elastic collision	-
2	$e+{{H}_{2}}\to e+H_{2}^{\text{*}}$	Excitation	14
3	$e+{{H}_{2}}\to e+H+H$	Dissociation	8.9
4	$e+{{H}_{2}}\to e+e+H_{2}^{+}$	Ionization	15.4

表2 表面反应的集合

Table 2 Collection of surface reactions

Num.	Surface reaction	Adhesion factor
1	$H_{2}^{\text{*}}+wall\to {{H}_{2}}$	1
2	$H+H+wall\to {{H}_{2}}$	1
3	$H_{2}^{+}+wall\to {{H}_{2}}$	1

图2 不同微波功率/腔室压强条件下, 反应器轴线方向上的基团分布

Fig. 2 Group distribution in the axial direction of the reactor under different microwave power/chamber pressure conditions (a) Electron number density distribution; (b) Atomic H number density distribution

表3 不同腔室压强下, 基片中心(r=0, z=0.5)与边缘(r=38.1, z=0.5)处的电子数密度ne和原子H数密度nH

Table 3 Electron number density ne and atomic H number density nH at the center (r=0, z=0.5) and edge (r=38.1, z=0.5) of the substrate under different chamber pressures

Chamber pressure/kPa	n_e/m⁻³		n_H/m⁻³
Chamber pressure/kPa	r=0, z=0.5	r=38.1, z=0.5	r=0, z=0.5	r=38.1, z=0.5
6	1.14×10¹⁷	1.96×10¹⁵	2.83×10²¹	1.26×10²¹
8	2.09×10¹⁷	3.18×10¹⁵	6.00×10²¹	2.02×10²¹
10	3.44×10¹⁷	4.63×10¹⁵	1.05×10²²	2.21×10²¹
12	4.97×10¹⁷	5.31×10¹⁵	1.51×10²²	1.67×10²¹

图3 金刚石薄膜的表面形貌、截面形貌及厚度分布

Fig. 3 Surface morphology, cross-sectional morphology and thickness distribution of the diamond film (a) Surface topography of a silicon substrate diamond film with inset illustrating the ideal diamond crystal profile when the growth parameter α is 2.9; (b) Surface profile of silicon substrate diamond film obtained by laser confocal microscope; (c) Cross-sectional morphology of the edge of the diamond film; (d) Thickness distribution of diamond film

图4 硅衬底金刚石膜的Raman光谱(a)、PL光谱(b)及XRD图谱(c)

Fig. 4 Raman spectrum (a), PL spectra (b) and XRD pattern (c) of diamond films on silicon substrate

图5 抛光后的硅衬底金刚石膜的实物图及AFM表面形貌

Fig. 5 Actual photographic and AFM morphology of polished diamond films on silicon substrate (a) Actual photographic; (b) AFM image

图6 薄膜弯曲度及应力测试结果

Fig. 6 Results of film bending and stress test (a) Test area of the film stress test system; (b) Bending test results of the monocrystalline silicon substrate; (c) Bending test results of the polished silicon substrate diamond film; (d) Internal stress of the diamond film calculated by the Stoney formula

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热管理用3英寸硅衬底金刚石薄膜的制备

Preparation of 3-inch Diamond Film on Silicon Substrate for Thermal Management

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