高品质CVD金刚石的合成及其在刻刀方面的应用研究
摘要
本文采用热阴极直流等离子体化学气相沉积(DC-PCVD)方法,以CH_4+H_2+CO_2为反应气体,合成出了高品质、生长速率快的金刚石厚膜。研究了CO_2流量对金刚石膜生长的影响,包括表面形貌、晶粒取向、膜的质量、应力和生长速率变化等。
研制了一种CVD金刚石石材刻刀,适合于花岗岩及硬质石材上小号字的雕刻。研究了切削速度、进给量、切削深度等因素对刻刀寿命的影响。分析了刻刀的磨损机理和磨损过程。
Diamond is an excellent material and has high application value. Natural diamond isexpensive that restricts its application. High quality CVD diamond has approached naturaldiamond in some physical and chemical properties. Because of its large-area flaky shape, CVDdiamond film is endowed more advantage in application. Research on diamond film’s growthproperties is a hot problem. Also, more and more researchers focus on diamond film’sapplication these years.
In this paper, we synthesized diamond films on Mo substrate with hot cathode DC plasmachemical vapor deposition method. CH_4,H_2 and CO_2 were used as gas source and their flowswere 8sccm, 200sccm and 0-2sccm, respectively. SEM、XRD and Raman were used tocharacteristic films’morphology, structure and quality. The results indicate: with the increase ofCO_2 flow, the film became dense; Without CO_2addition, the film had a (100) orientation. WhenCO_2 flow up to 2sccm, (111) orientation was dominating. In the middle, (110) orientation wasthe main film orientation. XRD verified the structure’s differences of all samples;Accompanying the increase of CO_2flow (0.5-2sccm), the I_(111)/ I_(220) ratio increased from 0.02 to5.26, that exceeded natural diamond standard power’s I_(111)/ I_(220) ratio (3.7); Without CO_2additionor CO_2flow is 0.5sccm, the film had a bad quality because the graphite existed in the film. Thegraphite peak that aligned at 1580cm-1 in Raman spectra disappeared when CO_2 flow exceed0.5sccm. As was also seen, the compressive stress changed to tensile stress when CO_2flow is0.89sccm and the growth rate decreased with the addition of CO_2. High quality diamond films’growth rate can reach 12um/h.
Additional, we designed and manufactured a kind of CVD diamond graver that can be usedcarving small words on the surface of granite. We design orthogonal experiment. The varianceanalysis of experimental results indicating: cutting speed had a very significant influence ongraver life. Feed rate had a significant influence on graver life except depth of cut. Multipleregression analysis is made to get experienced life equation. The main wear mechanism is abrasive wear. We put forward wear process thorough observing wear morphologies.
研制了一种CVD金刚石石材刻刀,适合于花岗岩及硬质石材上小号字的雕刻。研究了切削速度、进给量、切削深度等因素对刻刀寿命的影响。分析了刻刀的磨损机理和磨损过程。
Diamond is an excellent material and has high application value. Natural diamond isexpensive that restricts its application. High quality CVD diamond has approached naturaldiamond in some physical and chemical properties. Because of its large-area flaky shape, CVDdiamond film is endowed more advantage in application. Research on diamond film’s growthproperties is a hot problem. Also, more and more researchers focus on diamond film’sapplication these years.
In this paper, we synthesized diamond films on Mo substrate with hot cathode DC plasmachemical vapor deposition method. CH_4,H_2 and CO_2 were used as gas source and their flowswere 8sccm, 200sccm and 0-2sccm, respectively. SEM、XRD and Raman were used tocharacteristic films’morphology, structure and quality. The results indicate: with the increase ofCO_2 flow, the film became dense; Without CO_2addition, the film had a (100) orientation. WhenCO_2 flow up to 2sccm, (111) orientation was dominating. In the middle, (110) orientation wasthe main film orientation. XRD verified the structure’s differences of all samples;Accompanying the increase of CO_2flow (0.5-2sccm), the I_(111)/ I_(220) ratio increased from 0.02 to5.26, that exceeded natural diamond standard power’s I_(111)/ I_(220) ratio (3.7); Without CO_2additionor CO_2flow is 0.5sccm, the film had a bad quality because the graphite existed in the film. Thegraphite peak that aligned at 1580cm-1 in Raman spectra disappeared when CO_2 flow exceed0.5sccm. As was also seen, the compressive stress changed to tensile stress when CO_2flow is0.89sccm and the growth rate decreased with the addition of CO_2. High quality diamond films’growth rate can reach 12um/h.
Additional, we designed and manufactured a kind of CVD diamond graver that can be usedcarving small words on the surface of granite. We design orthogonal experiment. The varianceanalysis of experimental results indicating: cutting speed had a very significant influence ongraver life. Feed rate had a significant influence on graver life except depth of cut. Multipleregression analysis is made to get experienced life equation. The main wear mechanism is abrasive wear. We put forward wear process thorough observing wear morphologies.
引文
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[2] Salgueiredo E, Almeida F A, Amaral M et al. CVD micro / nanocrystalline diamond(MCD/NCD) bilayer coated odontological drill bits [J]. Diamond & Related Materials, 2009,18:264-270
[3] Yamamoto Akira, Nawachi Norio, Tsutsumoto Takahiro, et al. Pressure sensor using p-typepolycrystalline diamond piezoresistors [J]. Diamond & Related Materials, 2005, 14:657-660
[4] Katz A, Lee C H, Tai K L. Advanced metallization schemes for bonding of InP-based laserdevices to CVD-diamond heatsinks [J]. Materials Chemistryand Physics, 1994, 37:303-328
[5] Prins Johan F. Ion-implanted, shallow-energy, donor centres in diamond: the effect ofnegative electron affinity [J]. Nuclear Instruments and Methods in Physics Research A, 2003,514:69-78
[6] Jany C, Tardieu A, Gicquel A, et al. Influence of the growth parameters on the electricalproperties of thin polycrystalline CVD diamond films [J]. Diamond and Related Materials, 2000,9:1086-1090
[7] Lu F X , Guo H B, Guo S B et al. Magnetron sputtered oxidation resistant and antireflectionprotective coatings for freestanding diamond film IR windows [J]. Diamond & RelatedMaterials, 2009, 18:244-248
[8] Li Jingqi, Zhang Jihua, Guo Wantu et al. Optical brazing technique for bonding diamondfilms to zinc sulfide [J]. Diamond and Related Materials, 2002, 11:753-756
[9] Seoa Soo-Hyung, Shinb Wan-Chul, Park Jin-Seok. A novel method of fabricatingZnO/diamond/Si multilayers for surface acoustic wave (SAW) device applications [J]. ThinSolid Films, 2002, 416:190-196
[10] Castro G, Almeida F A, Oliveira F J, et al. Dry machining of silicon–aluminium alloys withCVD diamond brazed and directly coated Si3N4 ceramic tools [J]. Vacuum, 2008,82:1407-1410
[11] Almeida F A, A. Fernandes J S, Oliveira F J, et al. Semi-orthogonal turning of hardmetalwith CVD diamond and PCD inserts at different cutting angles [J]. Vacuum, 2009,83:1218-1223
[12] Liang Qi, Vohra Yogesh K, Thompson Raymond. High speed continuous and interrupteddry turning of A390 Aluminum/Silicon Alloyusing nanostructured diamond coated WC–6 wt.%cobalt tool inserts byMPCVD [J]. Diamond & Related Materials, 2008, 17:2041-2047
[13] Almeida F A, Sacramento J, Oliveira F J, et al. Micro- and nano-crystalline CVD diamondcoated tools in the turning of EDM graphite [J]. Surface & Coatings Technology, 2008,203:271-276
[14] Polini Riccardo, Bravi Fabio, Casadei Fabrizio, et al. Effect of substrate grain size andsurface treatments on the cutting properties of diamond coated Co-cemented tungsten carbidetools [J]. Diamond and Related Materials, 2002, 11:726-730
[15] Xu Zhenqing, Lev Leonid, Lukitsch Michael, et al. Effects of surface pretreatments on thedeposition of adherent diamond coatings on cemented tungsten carbide substrates [J].2007,16:461-466
[16]刘健敏. CVD金刚石薄膜在光电器件中的应用研究[D].上海:上海大学材料科学和工程学院, 2007.
[17] Oliveira Robson T S, Salazar-Banda Giancarlo R, Santos Mauro C, et al. Electrochemicaloxidation of benzene on boron-doped diamond electrodes [J]. Chemosphere, 2007,66:2152-2158
[18] Wang S G, Zhang Qing, Yoon S F, et al. Electron field emission enhancement effects ofnano-diamond films [J]. Surface and Coatings Technology, 2003, 167:143-147
[19] Roos M, Baranauskas V, Fontana M, et al. Electron field emission from boron dopedmicrocrystalline diamond [J]. Applied Surface Science, 2007, 253:7381-7386
[20] Xu Junqi, Fan Huiqing, Liu Weiguo, et al. Large-area uniform hydrogen-free diamond-likecarbon films prepared by unbalanced magnetron sputtering for infrared anti-reflection coatings[J] . Diamond & Related Materials, 2008, 17:194-198
[21] Matsumoto S, Sato Y, TsuTsumi M, et al. Growth of diamond particals frommethane-hydrogen gas [J]. J.Mater.Sci, 1982, 17(11):3106-3112
[22] Pecoraro S, Arnault J C, Werckmann J. BEN-HFCVD diamond nucleation on Si(111)investigated by HRTEM and nanodiffraction [J]. Diamond & Related Materials, 2005,14:137-143
[23] Kamo Mutsukazu, Sato Yoichiro, Matsumoto Seiichiro, et al. Diamond synthesis from gasphase in microwave plasma [J]. Volume, 1983, 62:642-644
[24] Liang Qi, Chin Cheng Yi, Lai Joseph, et al. Enhanced growth of high quality single crystaldiamond by microwave plasma assisted chemical vapor deposition at high gas pressures [J].APPLIED PHYSICS LETTERS, 2009, 94:024103
[25]Sternschulte H, Thonke K, Munzinger P C, et al. 1.681-eV luminescence center inchemical-vapor-deposited homoepitaxial diamond films [J]. Phys. Rev. B, 1994,50:14554-14560
[26]Bai Y Z, Jiang Z G, Wang C L, et al. Effects of alcohol addition on the deposition ofdiamond thick films by dc plasma chemical vapor deposition method [J]. Chinese PhysicsLetters, 1998, 15:228-229
[27] Jing Z S, Jiang Z G, Bai Y Z, et al. Synthesis of Thick Diamond Film by Direct CurrentHot-Cathode Plasma Chemical Vapor Deposition [J].Chinese Physics Letters, 2002,19:1374-1376
[28] Guo H, Sun Z L, He Q Y, et al. Deposition of large area high quality diamond wafers withhigh growth rate byDC arc plasma jet [J]. Diamond and Related Materials, 2000, 9:1673-1677
[29] Kawarada H, Mar K S, Hiraki A. Large area chemical vapour deposition of diamondparticles and films using magneto-microwave plasma[J].Jpn.J.Appl.Phys,1987,26:L1032-L1034
[30]姜志刚.高气压直流辉光放电及其等离子体化学气相沉积金刚石厚膜的生长特性与应用研究[D].吉林:吉林大学原子与分子物理研究所, 2004
[31] Wang Z L, Lu C, Li J J, et al. Effect of gas composition on the growth and electricalproperties of boron-doped diamond films [J]. Diamond & Related Materials, 2009, 18:132-135
[32]吕江维,冯玉杰,彭鸿雁等.硼掺杂对直流热阴极CVD金刚石薄膜生长特性的影响[J].无机材料学报,2009, 24:607-611
[33] Sebert W M, Worner E ,Fuchs F , et al. Nitrogen induced increase of growth rate inchemical vapor deposition of diamond [J]. Appl. Phys. Lett, 1996, 68:759-760
[34] Smith J A, Rosser K N, Yagi1H, et al. Diamond deposition in a DC-arc Jet CVD system:investigations of the effects of nitrogen addition [J]. Diamond and Related Materials, 2001,10:370-375
[35] Bénédic F, Belmahi M, Elmazria O, et al. Investigations on nitrogen addition in the CH4–H2gas mixture used for diamond deposition for a better understanding and the optimisation of thesynthesis process [J]. Surface and CoatingsTechnology, 2003, 176:37-49
[36] Tang C J, Pereira S M S, Fernandes AJ S, et al. Synthesis and structural characterization ofhighly <100> oriented {100}-faceted nanocrystalline diamond films by microwave plasmachemical vapor deposition [J]. Journal of Crystal Growth, 2009, 311:2258-2264
[37] Yu Z, Karlsson U, Flodstr?m A. Influence of oxygen and nitrogen on the growth ofhot-filament chemical vapor deposited diamond films [J]. Thin Solid Films, 1999, 342:74-82
[38] Sun B, Zhang X, Lin Z. Growth mechanism and the order of appearance of diamond (111)and (100) facets [J]. Phys. Rev. B, 1993, 47:9816-9824
[39] Elliott M A, May P W, Petherbridge J, et al. Optical emission spectroscopic studies ofmicrowave enhanced diamond CVD using CH4/CO2 plasmas [J]. Diamond and related materials,2000, 9:311-316
[40] Petherbridge J, May P W, Pearce S R J, et al. Molecular beam mass spectrometryinvestigations of low temperature diamond growth using CO2 /CH4 plasmas [J]. Diamond andrelated materials, 2001, 10:393-398
[41] Ando Yutaka, Tachibana Takeshi, Kobashi Koji. Growth of diamond films by a 5-kWmicrowave plasma CVD reactor [J]. Diamond and related materials, 2001, 10:312-315
[42] Gu Changzhi, Jin Zengsun, Wang Chunlei, et al. Growth of (100) orientation diamond filmdeposited by MWPCVD methods using the gaseous mixtures of CH4, CO and H2[J]. Diamondand related materials, 1998, 7:765-768
[43] Bougdira Jamal, Remy Michel, Alnot Patrick, et al. Combined effect of nitrogen and pulsedmicrowave plasma on diamond growth using CH4–CO2gas mixture [J]. Thin Solid Films, 1998,325:7-13
[44] Itoh Ken-ichi, Matsumoto Osamu. Diamond deposition procedure from microwave plasmasusing a mixture of CO2-CH4 as carbon source [J] . Thin Solid Films, 1998, 316:18-23
[45] Wild C, Koidl P, Müller-Sebert W, et al. Chemical vapour deposition and characterizationof smooth {100}-faceted diamond films [J]. Diamond and Related Materials, 1993, 2:158-168
[46] Michler J, Mermoux M, von Kaenel Y, et al. Residual stress in diamond films: origins andmodeling [J]. Thin Solid Films, 1999, 357:189-201
[47] Nakamur Y, Mermoux M, Kaenel Y von, et al. Measurement of internal stresses in CVDdiamond films [J]. 1997, 308-309:249-253
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