类金刚石微球的高温高压制备

韩晶晶; 贺端威; 马迎功; 丁未; 芶立; 唐永建

doi:10.11858/gywlxb.2017.03.002

类金刚石微球的高温高压制备

doi: 10.11858/gywlxb.2017.03.002

韩晶晶^1,,
贺端威^1,*, ,,
马迎功¹,
丁未¹,
芶立²,
唐永建³

1.
四川大学原子与分子物理研究所，四川成都 610065
2.
四川大学材料科学与工程学院，四川成都 610065
3.
中国工程物理研究院激光聚变研究中心，四川绵阳 621999

详细信息

作者简介:
韩晶晶(1989—), 女，硕士，主要从事大腔体静高压技术和高压材料物性研究. E-mail:714753083@qq.com

通讯作者:
贺端威(1969—), 男，博士，教授，博士生导师，主要从事高压科学与技术、超硬材料及纳米材料的研究. E-mail:duanweihe@scu.edu.cn

中图分类号: O521.2
计量
- 文章访问数: 5980
- HTML全文浏览量: 2636
- PDF下载量: 73
出版历程
- 收稿日期: 2016-03-29
- 修回日期: 2016-10-12

Synthesis of Diamond-Like Carbon Spheres under High Temperature and High Pressure

1.
Institute of Atomic and Molecular Physics, Sichuan University, Chengdu 610065, China
2.
College of Materials Science and Engineering, Sichuan University, Chengdu 610065, China
3.
Research Center of Laser Fusion, China Academy of Engineering Physics, Mianyang 621999, China

摘要

摘要: 通过对化学气相沉积方法获得的碳膜微球进行高温高压处理，在约8 GPa、1 600 ℃的条件下制备了类金刚石异质实心微球样品，芯轴为钼球。根据金刚石和钼的体积随压力及温度的变化规律，设计并优化了样品制备的温度-压力路径，以降低因类金刚石膜层与钼球的体弹模量及热膨胀系数差异而导致的残余应力。拉曼光谱测试结果表明，样品膜层具有明显的1 332 cm^-1金刚石特征峰，高温高压有效地消除了存在于初始碳膜微球中的反式聚乙炔，同时降低了膜中残余应力，产生了有利于提高类金刚石膜强度的压应力；扫描电子显微镜测试结果表明，样品球形度良好，平均直径约2 mm，类金刚石膜表面平均晶粒尺寸约为100 nm，膜厚约为20 μm；原子力显微镜测试结果表明，类金刚石膜层的表面粗糙度为647 nm。
- 类金刚石微球 /
- 高温高压 /
- 残余应力
Abstract: Carbon microspheres prepared using the chemical vapor deposition method were treated under high-pressure and high-temperature conditions of about 8 GPa and 1 600 ℃.Based on the volume variation of diamond and molybdenum with the pressure and temperature, we designed and optimized the temperature-pressure path for sample treatments, thereby reducing the residual stress caused by the difference between the diamond's and the molybdenum's elastic modulus and thermal expansion.The Raman spectrum show that the samples have an obvious 1 332 cm^-1 diamond characteristic peak, and the high-temperature and high-pressure treatments effectively eliminate the trans-polyacetylene in the initial diamond-like carbon microsphere.The scanning electron microscope results show that the samples exhibit good sphericity, with an average diameter of 2 mm, the diamond-like film surface has an average grain size of 100 nm, and the film thickness is about 20 μm.The atomic force microscope test results show that the surface roughness is 647 nm.
- diamond-like microspheres /
- high-temperature and high-pressure treatment /
- residual stress

HTML全文

图 1 类金刚石膜于钼球表面脱落

Figure 1. Delamination of diamond-like film on molybdenum sphere

下载: 全尺寸图片幻灯片

2(a) 金刚石和钼的相对体积(V₀/V)随压力(p)的变化

2(a). Relative volume (V₀/V) variation of diamond and molybdenum with pressure (p)

下载: 全尺寸图片幻灯片

2(b) 金刚石和钼的相对体积(V₀/V)随温度(T)的变化

2(b). Relative volume (V₀/V) variation of diamond and molybdenum with temperature (T)

下载: 全尺寸图片幻灯片

图 3 高温高压处理的温度-压力路径设计

Figure 3. Designed high-temperature and high-pressure path for sample treatments

下载: 全尺寸图片幻灯片

4(a) 高温高压处理后微球样品的扫描电镜全貌图

4(a). Scanning electron microscope image of microsphere after high-temperature and high-pressure treatment

下载: 全尺寸图片幻灯片

4(b) 空心类金刚石微球球壳的扫描电镜全貌图

4(b). Scanning electron microscope image of hollow diamond-like spherical shell

下载: 全尺寸图片幻灯片

图 5 样品扫描电镜照片

Figure 5. Scanning electron micrographs of samples

下载: 全尺寸图片幻灯片

6(a) 初始微球表面的拉曼光谱

6(a). Raman spectrum of surface of initial microspheres

下载: 全尺寸图片幻灯片

6(b) 高温高压处理后微球表面的拉曼光谱

6(b). Raman spectrum of surface of microspheres after high-temperature and high-pressure treatment

下载: 全尺寸图片幻灯片

图 7 样品表面原子力显微镜测试结果

Figure 7. Atomic force microscope result of sample surface

下载: 全尺寸图片幻灯片

参考文献(29)

[1]	AISENBERG S, CHABOT R.Ion-beam deposition of thin films of diamondlike carbon[J].J Appl Phys, 1971, 42(7):2953-2958. doi: 10.1063/1.1660654
[2]	CONWAY N M J, MILINE W I, ROBERSTON J.Electronic properties and doping of hydrogenated tetrahedral amorphous carbon films[J].Diam Relat Mater, 1998, 7(2):477-481. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=4092df9cf629e16076ca89fbd6b75686
[3]	DEKEMPENEER E H A, JACOBS R, SMEETS J, et al.R.f.plasma-assisted chemical vapor deposition of diamond-like carbon:physical and mechanical properties[J].Thin Solid Films, 1992, 217(1/2):56-61. https://www.sciencedirect.com/science/article/pii/004060909290605B
[4]	LACERDA R G, MARQUES F C.Hard hydrogenated carbon films with low stress[J].Appl Phys Lett, 1998, 73(5):617-619. doi: 10.1063/1.121874
[5]	LIFSHITZ Y.Diamond-like carbon-present status[J].Diam Relat Mater, 1999, 8(8/9):1659-1676. http://d.old.wanfangdata.com.cn/NSTLQK/NSTL_QKJJ025135161/
[6]	BARANOV A M, VARFOLOMEEV A E, NEFEDOV A A, et al.Development of DLC film technology for electronic application[J].Diam Relat Mater, 2000, 9(3):649-653. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=40259a7eb4b8122dde9c9c35616fcfd5
[7]	ROBERTSON J.Diamond-like amorphous carbon[J].Mater Sci Eng R, 2002, 37(4):129-281. http://d.old.wanfangdata.com.cn/Periodical/gsyxb200505006
[8]	LINDL J D, AMENDT P, BERGER R L, et al.The physics basis for ignition using indirect-drive targets on the National Ignition Facility[J].Phys Plasmas, 2004, 11(2):339-480. doi: 10.1063/1.1578638
[9]	BIENER J, MIRARIMI P B, TRINGE J W, et al.Diamond ablators for inertial confinement fusion[J].Fusion Sci Technol, 2006, 49(4):737-742. doi: 10.13182/FST49-737
[10]	ROSS J S, HO D, MILOVICH J, et al.High-density carbon capsule experiments on the national ignition facility[J].Phys Rev E, 2015, 91(2):021101. doi: 10.1103/PhysRevE.91.021101
[11]	MACKINNON A J, MEEZAN N B, ROSS J S, et al.High-density carbon ablator experiments on the National Ignition Facility[J].Phys Plasmas, 2014, 21(5):056318. doi: 10.1063/1.4876611
[12]	DAWEDEIT C, KUCHEYEV S O, SHIN S J, et al.Grain size dependent physical and chemical properties of thick CVD diamond films for high energy density physics experiments[J].Diam Relat Mater, 2013, 40:75-81. doi: 10.1016/j.diamond.2013.10.001
[13]	BIENER J, HO D D, WILD C, et al.Diamond spheres for inertial confinement fusion[J].Nucl Fusion, 2009, 49(11):112001. doi: 10.1088/0029-5515/49/11/112001
[14]	李晨.金刚石膜的应力研究[D].长春: 长春理工大学, 2009: 8-40. http://www.wanfangdata.com.cn/details/detail.do?_type=degree&id=Y1524610 LI C.Investigation of stress in diamond films[D].Changchun: Changchun University of Science and Technology, 2009: 8-40. http://www.wanfangdata.com.cn/details/detail.do?_type=degree&id=Y1524610
[15]	龙芬.Mo箔基体上金刚石薄膜的制备及残余应力的研究[D].长沙: 中南大学, 2014: 11-51. http://cdmd.cnki.com.cn/Article/CDMD-10533-1014408457.htm LONG F.Study of preparation and residual stress of diamond films on Mo foil[D].Changsha: Zhongnan Univesity, 2014: 11-51. http://cdmd.cnki.com.cn/Article/CDMD-10533-1014408457.htm
[16]	WANG Y K, YIN S, LEI L, et al.Enhanced hardness of CVD diamond after high pressure and high-temperature treatments[J].High Pressure Res, 2015, 35(4):363-371. doi: 10.1080/08957959.2015.1096933
[17]	DEWAELE A, DATCHI F, LOUBEYRE P, et al.High pressure-high temperature equations of state of neon and diamond[J].Phys Rev B, 2008, 77(9):094106. doi: 10.1103/PhysRevB.77.094106
[18]	ZHAN Y S, LAWSON A C, ZHANG J Z, et al.Thermoelastic equation of state of molybdenum[J].Phys Rev B, 2000, 62(13):8766-8776. doi: 10.1103/PhysRevB.62.8766
[19]	SLACK G A, BARTRAM S F.Thermal expansion of some diamondlike crystals[J].J Appl Phys, 1975, 46(1):89-98. doi: 10.1063/1.321373
[20]	BIRCH F.Finite elastic strain of cubic crystals[J].Phys Rev, 1947, 71(11):809-824. doi: 10.1103/PhysRev.71.809
[21]	于白茹.金刚石、氮化硼、氧化铍高压物性的第一性原理计算[D].成都: 四川大学, 2010: 50-55. YU B R.First-principles calculations for properties of diamond, BN and BeO under high pressure[D].Chengdu: Sichuan University, 2010: 50-55.
[22]	曾召益.过渡金属钼、镍钛合金的高压相变及热力学性质研究[D].成都: 四川大学, 2011: 62-65. ZENG Z Y.Phase transition and thermodynamic properties of Mo and NiTi alloy under high pressures[D].Chengdu: Sichuan University, 2011: 62-65.
[23]	王海阔, 贺端威, 许超, 等.基于国产铰链式六面顶压机的大腔体静高压技术研究进展[J].高压物理学报, 2013, 27(5):633-661. http://www.gywlxb.cn/CN/abstract/abstract1618.shtml WANG H K, HE D W, XU C, et al.Development of large volume-high static pressure techniques based on the hinge-type cubic presses[J].Chinese Journal of High Pressure Physics, 2013, 27(5):633-661. http://www.gywlxb.cn/CN/abstract/abstract1618.shtml
[24]	GLIKES K W R, PRAWER S, NUGENT K W, et.al.Direct quantitative detection of the sp³ bonding in diamond-like carbon films using ultraviolet and visible Raman spectroscopy[J].J Appl Phys, 2000, 87(10):7283-7289. doi: 10.1063/1.372981
[25]	FERRARI A C, ROBERTSON J.Interpretation of Raman spectra of disordered and amorphous carbon[J].Phys Rev B, 2000, 61(20):14095-14107. doi: 10.1103/PhysRevB.61.14095
[26]	KNIGHT D S, WHITE W B.Characterization of diamond films by Raman spectroscopy[J].J Mater Res, 1989, 4(2):385-393. doi: 10.1557/JMR.1989.0385
[27]	FERRARI A C, ROBERTSON J.Raman spectroscopy of amorphous, nanostructured, diamond-like carbon, and nanodiamond[J].Phil Trans R Soc A, 2004, 362:2477-2512. doi: 10.1098/rsta.2004.1452
[28]	WINDISCHMANN H, GRAY K J.Stress measurement of CVD diamond films[J].Diam Relat Mater, 1995, 4:837-842. doi: 10.1016/0925-9635(94)05327-8
[29]	赵南方, 杨巧勤, 赵立华.热丝CVD法金刚石薄膜宏观内应力分析[J].矿业工程, 1998, 18(3):67-69. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=QK199800364701 ZHAO N F, YANG Q Q, ZHAO L H, et al.Intrinsic stress in diamond film growth by hot-filament CVD[J].Mining and Metallurgical Engineering, 1998, 18(3):67-69. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=QK199800364701