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Chemical Vapor Deposition of Boron and Boron Nitride from Decaborane(L4) A)

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Chemical Vapor Deposition of Boron and Boron Nitride from Decaborane(L4) A) University of Nebraska - Lincoln DigitalCommons@University of Nebraska - Lincoln Peter Dowben Publications Research Papers in Physics and Astronomy July 1989 Chemical vapor deposition of boron and boron nitride from decaborane(l4) a) Yoon Gi Kim Syracuse University Peter A. Dowben University of Nebraska-Lincoln, [email protected] J.T. Spencer Syracuse University G.O. Ramseyer General Electric Company Follow this and additional works at: https://digitalcommons.unl.edu/physicsdowben Part of the Physics Commons Gi Kim, Yoon; Dowben, Peter A.; Spencer, J.T.; and Ramseyer, G.O., "Chemical vapor deposition of boron and boron nitride from decaborane(l4) a)" (1989). Peter Dowben Publications. 134. https://digitalcommons.unl.edu/physicsdowben/134 This Article is brought to you for free and open access by the Research Papers in Physics and Astronomy at DigitalCommons@University of Nebraska - Lincoln. It has been accepted for inclusion in Peter Dowben Publications by an authorized administrator of DigitalCommons@University of Nebraska - Lincoln. Skuilna, van der Leeden, and Vincent: Calibration of an argon in germanium standard *G. C. Schwartz and R. E. Jones, IBM J. Res. Dev. 14,52 (1970). "W. K. Chu, J. W. Mayer, and M. A. Nicolet, BackrcatteringSpectrometry 3K.Tanaka, S. Yamasaki, K. Nakagawa, A. Matsuda, H. Okushi et ol., J. (Academic, New York, 1978). Non-Cryst. Solids 35/36,475 (1980). I2P. R. Bevington, Data Reduction and Error Anolysisfor rhe Physical Sci- 'H. F. Winters and E. Kay, J. Appl. Phys. 38,3928 (1967). ences ( McGraw-Hill, New York, 1969 ) . 'K. M. Skulina, Ph.D. thesis, The University of Michigan, 1988. I3J. F. Ziegler, Helium, Stopping Pourers and Ranges in All Elemental Mot- 'C. J. Fang, K. J. Gruntz, L. Ley, M. Cardona, F. J. Demond erol., J. Non- ter, VoL 4 of Stopping ond Ranges of Ions in Morrer (Pergamon, New Cryst. Solids 35/36,255 ( 1980). York, 1977). 'K. M. Skulina, G. A. van der Leeden, D. H. Vincent, and R. T. Young (to I4M. H. Brodsky, D. Kaplan, and J. F. Ziegler, Appl. Phys. Lett. 21, 305 be published). (1972). 'L. R. Doolittle, Nucl. Instrum. Methods B 9, 344 (1985). I5J. I. Goldstein, D. E. Newbury, P. Echlin, D. C. Joy, C. Fiori, and E. 9L.R. Doolittle, Nucl. Instrum. Methods B 15, 227 (1986). Lifshin, "Quantitative X-Ray Microanalysis," in Scanning Electron Mi- ''A. Savitsky and M. J. E. Golay, Anal. Chem. 36, 1627 (1064). croscopy ond X-Roy Micrwnolysis (Plenum, New York, 198 l ). Chemical vapor deposition of boron and boron nitride from decaborane(l4)8) Yoon Gi Kim, P. A. Dowben, and J. T. Spencer Centerfor Molecular Electronics, Departments of Physics and Chemistry, Syracuse University, Syracuse, New York 13244-1 130 G. 0. Ramseyer Electronics Laboratory, General Electric Company, Electronics Park, P. 0.Box 4840, Syracuse, New York 13221 (Received 30 October 1988; accepted 28 January 1989) We have investigated photoassisted, plasma enhanced chemical vapor deposition and pyrolytic deposition of boron from decaborane (BloH14)and boron nitride from decaborane combined with nitrogen or ammonia. The use of decaborane for depositing boron and boron nitride thin films is seen as a viable alternative to diborane or boron halides. I. INTRODUCTION II. EXPERIMENTAL The formation of cubic boron nitride has been intensively Decaborane( l4), BloH14,is an air-stable white crystalline investigated,'-9 motivated by this material's potential as a solid with a vapor pressure of several Torr at room tempera- hard coating, which arises from the large cohesive energy t~re.~~The vapor pressure can be readily raised by heating and hardness of BN. It also has been noted that BN is not decaborane (the vapor pressure at 100 "C is 19 Torr), since only useful in the manufacturing of hard cutting tools, but the molecule decomposes only above 170 0C.36The decabor- because of the excellent insulating dielectric properties and ane( 14) was sublimed to separate the material from cellite corrosion resistant nature of BN, thin films of BN could be (a stabilizer) and other impurities. The radio-frequency useful for the fabrication of insulated conductors, capaci- plasma deposition studies were carried out in a small 3-in., tors, and providing hard protective coatings for diodes, tran- 13.56-kHz rf plasma reactor with a 1-in. plate separation. sistors, and other monolithic devices. ''-I2 Boron source ma- The typical power consumption of the reactor was 20 W, but terials useful for fabricating BN thin films may also be could be increased to 100 W. The sample was mounted on valuable for doping semiconductor materials with boron do- the ground plate of the two-plate system, with the other plate pant atoms. ','I4 connected to the rfnetwork. The system used a commercial With these substantial applications for depositing BN thin rf generator and impedance matcher. Argon was used as a films and boron dopant atoms, a number of boron source carrier gas for pure boron deposition studies, while 300-500 compounds have been employed including BC13,2.7.8.'0,'5-22 p NH, or N, was employed when boron nitride deposition BF3,23diborane (B2H,),2.3-9.1 1.24-29 trichlor~borazole,~~tri- was sought. The carrier gas was mixed with the BlOHl4va- methoxyborozole, l2 trimethy lboron, l3 boric acid por prior to admission to the rf plasma reactor. The carrier (H3B03),31 HB02,'4-32 borazine B,N,H, (Refs. 2,3,33, and gas pressures, as well as that for Bl0H,,, were controlled by 34), as well as evaporated b~ron.~.'~With the goal of the stainless-steel needle valves and monitored by thermocouple deposition of pure boron or boron nitride, many of these gauges. The Bl0H,, source vessel was heated to 80 "C to in- source compounds have serious defects, including serious crease the decaborane( 14) vapor pressure. All depositions safety problems due to the toxicity and/or highly inflamma- were carried out with a constant gas flow to ensure sample ble nature of the source compounds. We have explored the purity. Typically, a Bl0H,, pressure of 10 to 50 p was ad- deposition of boron and boron nitride using decaborane mitted to the rf plasma reactor ( 10 p for BN and 50 p for (B,,H as a source material. B4N). 2796 J. Vac. Sci. Technol. A 7 (4), Jul/Aug 1989 0734-2101/89/042796-04$01.00 @ 1989 American Vacuum Society 2796 2797 Kim etaL: CVD of boron and boron nitride from decaborane(l4) 2797 The photodeposition of boron and boron nitride was un- formation of pure boron nitride with both nitrogen and am- dertaken using a Quantel International Nd:YAG laser oper- monia as the ambient background gas. ating at 532 nm, with a pulse length of 10 ns and a peak Since decaborane contains no organic ligands or oxygen, power of 124 mJ/pulse. Pyrolysis was undertaken with a deposition of pure boron or boron nitride is limited only by flow regime in a glass vacuum system described else- the residual impurities of the vacuum system and the source here.,^.,^ Temperature was determined using a Chroml- materials. As can be seen in Fig. 1, even boron-nitrogen Alumel thermocouple spot welded to a resistively heated films with high concentrations of boron are observed to con- nickel foil. tain little or no oxygen or carbon when made from the plas- ma assisted deposition of BloHl, in NH, or N,. Elemental analysis of boron rich plasma deposited films (B:N ratios of Ill. RESULTS AND DISCUSSION 5: 1) did find substantial hydrogen incorporation in the film With a substantial (50p) decaborane( 14) pressure, pyro- ( - 6.6%) which may be the result of the incomplete disso- lysis of BloH14on a nickel foil was not observed to occur ciation of the decaborane( 14). below 580 "C. At 600 "C, BloH14will pyrolyze at a sufficient- Ion beam assisted decomposition of borazine3, has been ly fast rate so that in a N, ambient atmosphere, complete successfully employed to deposit cubic boron nitride, but the nitride formation did not occur and the nitrogen concentra- use of borazine makes the film composition difficult to con- tion within the film did not exceed 3%. These pyrolysis tem- trol. By varying the relative BloH14to NH, or N, concentra- peratures are substantially lower than the temperatures of tion, the composition of the film can be altered as shown in 600 to 1000 "C commonly used in the pyrolysis of dibor- Fig. 2. To deposit the films shown, - 50-p decaborane and ane(6),"~~~,~~1500 to 1800 "C used with 1,3,5 trimethoxy- 400-600 p of N, was admitted to the rf reactor chamber. borazoleI2 and 1100 to 2300 "C with boron tri~hloride.'.~~ Boron-nitrogen films with very low concentrations of nitro- The temperature used for pyrolysis of decaborane was com- gen will, however, readily react in air, heavily oxidizing the parable with the pyrolysis temperature of 300-650 "C used film as seen in Fig. 1. with b~razine,~and some results reported for diborane(6) Since the decomposition of BlOHl4can be a surface medi- and NH, mixtures28in the 400-700 "C temperature range. ated reaction, as demonstrated by our pyrolytic studies, spe- With plasma assisted deposition processes, the thermal cially localized deposition of boron or boron nitride can energies necessary for pyrolysis are substituted with electron therefore be accomplished either by photoassisted or elec- kinetic energies (the electron kinetic energies run from 10 to tron assisted decomposition of the absorbed BloH14species 100 eV or the temperature equivalent of lo4 to 10' K) and at substrate temperatures (for nickel) below 580 "C. To consequently, the substrate temperature can be much re- demonstrate that photoassisted patterned deposition of bo- d~ced.~~-~'Boron deposition on GaAs substrates was ob- ron nitride and boron could be undertaken employing deca- served with rf plasma assisted deposition at substrate tem- borane as a source material, we deposited boron on GaAs perature below 242 "C with the reactor operating at 20-W substrates (at room temperature) using a close contact mask power.
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