CVD Gas-Phase Analysis using In Situ Molecular-Beam Mass Spectrometry

Some of the earliest diagnostic work we did in the mid 1990s involved using a molecular-beam mass spectrometer to sample gases from diamond reactors during the CVD process. This is particularly tricky to do, as the CVD process pressure is typically a few 10s of torr, while the mass spectrometer operates at ~10-8 torr.
A Quadrupole Mass spectrometer (Hiden Analytical), samples gas from a hot filament reactor through a 100-µm-diameter orifice. The gas passes from the reaction chamber at 20 Torr into a differentially-pumped region at 1mTorr, and forms a molecular beam. This beam then enters another orifice which is the entrance to the mass spectrometer at 10-8 Torr. Thus, molecules which pass through both holes are then in a UHV region with a very large mean free path, and can travel to the detector without undergoing any collisions. This effectively freezes out any chemical reactions, allowing highly reactive species, such as hydrocarbon radicals, ions and atoms to be detected. Mechanically chopping the beam, and using phase sensitive detection allows increased sensitivity.Recently we have done work studying standard CH4/H2 gas mixtures, as well as looking at the effect upon the chemistry, and the diamond film, of additions of chlorine- nitrogen and phosphorus-containing gases.
Related Papers
- P.W. May, C.A. Rego, R.G. Thomas, M.N.R. Ashfold, K.N. Rosser, P.G. Partridge and N.M. Everitt, "Preparation of CVD Diamond Wires, Fibres and Tubes", Proc. 3rd Int. Symp. Diamond Mater., Honolulu, Hawaii, 1993, Proceedings Volume PV 93-17, edited by J.P. Dismukes and K.V. Ravi (Electrochem. Soc, Pennington, NJ), pp.1036-1041.
- P.W. May, C.A. Rego, R.M. Thomas, M.N.R. Ashfold, K.N. Rosser, P.G. Partridge and N.M. Everitt, "Preparation of Solid and Hollow Diamond Fibres and the Potential for Diamond Fibre Metal Matrix Composites", J. Mater. Sci. Lett., 13 (1994) 247-9.
- P.W. May, C.A. Rego, R.M. Thomas, M.N.R. Ashfold, K.N. Rosser and N.M. Everitt, "CVD Diamond Wires and Tubes", Diamond Rel. Mater., 3 (1994) 810-813.
- P.G. Partridge, P.W. May and M.N.R. Ashfold, "Chemical Vapour Deposited Diamond Fibres: Manufacture and Potential Properties", Mater. Sci. Technol., 10 (1994) 177-189.
- P.W. May, C.A. Rego, M.N.R. Ashfold, K.N. Rosser, G. Lu, T.D. Walsh, L. Holt, N.M. Everitt and P.G. Partridge, "CVD Diamond-Coated Fibres", Diamond Rel. Mater., 4 (1995) 794-797
- P.G. Partridge, M.N.R. Ashfold, P.W. May and E.D. Nicholson, "The Effective Chemical Vapour Deposition Rate of Diamond", J. Mater. Sci., 30 (1995) 3973-3982.
- G.H. Lu, P.G. Partridge and P.W. May, "A Technique for the Manufacture of Long Hollow Diamond Fibres by Chemical Vapour Deposition", J. Mater. Sci. Lett., 14 (1995) 1448-1450.
- E.D Nicholson, J.E Field, P.G Partridge, M.N.R. Ashfold, "The Mechanical Properties of Diamond Films, and Diamond-Coated Fibres and Wires", Mater. Res. Soc. Symp. Proc. 383 (1996) 101-113.
- N.M. Everitt, R.A. Shatwell, E. Kalaugher and E.D. Nicholson, "Mechanical Properties of Diamond Fibres", Mater. Res. Soc. Symp. Proc. 383 (1996) 379-384.
- G. Meaden, P. G. Partridge, M.N.R Ashfold, E.D Nicholson, A Wisbey, "Laser Cutting of Diamond Fibres and Diamond Fibre/Titanium Metal Matrix Composites", Diamond Relat. Mater. 5 (1996) 825
- E.D Nicholson, T.W. Baker, S.A. Redman, E. Kalaugher, K.N. Rosser, N.M. Everitt, M.N.R. Ashfold and P.G. Partridge, "Young's modulus of diamond-coated fibres and wires", Diamond Relat. Mater. 5 (1996) 658.
- E.D. Nicholson, J.R. Weeks and M.N.R. Ashfold "The Effect of varying Deposition Conditions on the Young's Modulus of Diamond-Coated Wires", Diamond Relat. Mater. 6 (1997) 817.
- E. Kalaugher, N.M. Everitt and E.D. Nicholson "Factors Affecting the Fracture Strength and Young's Modulus of CVD Diamond-Coated Fibres", Diamond Relat. Mater. 6 (1997) 826
- P.G. Partridge, A. Fookes, E.D. Nicholson, T. Pearce and G. Meaden "Nanoscale Grinding of Ceramics using Diamond Fibres", Diamond Relat. Mater. 6 (1997) 893
- N.P. Smith, M.N.R. Ashfold, D.J. Smith and T.R.A. Pearce, "Manufacture and Performance of Diamond-Coated Thermocouples", Diamond Relat. Mater., 8 (1999) 956-960.