Abstract

ZnSe crystals were grown by self-seeded physical vapor transport (PVT) technique in the horizontal configuration. The source materials were heat treated by H₂ reduction to remove the oxides followed by baking under dynamic vacuum to adjust the source composition toward that of congruent sublimation. Contactless growth of ZnSe single crystals have been performed using three different source materials. The crystals grew away from the ampoule wall with large (1 1 0) facets tending to align parallel to the gravity direction. The SEM micrographs and the AFM images showed that large (1 1 0) terraces and steps dominate the as-grown facets. The measured residual gas pressure and composition (mostly CO and H₂) in the processed ampoules were similar for all source materials used. One-dimensional diffusion model on the mass flux of a multi-species PVT system was employed to analyze the conditions for contactless growth. The calculated thermal profile for supersaturation is very close to the thermal profile measured inside the empty furnace bore in the region of contactless growth. The effects of convective flows in the vapor phase inside the ampoule on the growth processes are discussed.

Author Keywords: Contactless growth; Physical vapor transport; Zinc selenide; Atomic force microscopy

PACS classification codes: 61.10

Article Outline

1. Introduction

2. Experimental procedure

2.1. Ampoule preparation and heat treatments of starting materials

2.2. Crystal growth experiments

2.3. Residual gas measurements and crystal characterization

3. Results and discussion

3.1. Morphology of grown crystals

3.2. Residual gas pressures and compositions

3.3. Supersaturation and growth directions

3.4. One-dimensional diffusion analysis

4. Conclusions

Acknowledgements

References

(45K)
Fig. 1. As-grown ZnSe crystals inside the ampoules. (a) ZnSe-39, (b) ZnSe-43 and (c) ZnSe-44. Gravity vector out of paper for (a) and into paper for (b) and (c).

(24K)
Fig. 2. Side views of the as-grown ZnSe-45 crystal. Gravity vector upward for (a) and downward for (b).

(28K)
Fig. 3. AFM height image (a), and a three-dimensional image (b) on the as-grown (1 1 0) facet of the ZnSe-39 crystal.

(13K)
Fig. 4. AFM three-dimensional image showing the step edge on the as-grown (1 1 0) facet of the ZnSe-39 crystal.

(3K)
Fig. 5. Growth directions of the self-seeded grown crystals.

(4K)
Fig. 6. The measured thermal profile (solid curve) and the calculated T_{supersaturation} profile (dotted curve) at the end of the ZnSe-42 run.

Table 1. The vendor of source material, the amount of ZnSe loaded and the condition of H₂ and vacuum baking heat treatments for each growth run (<1K)

Table 2. The source temperature, T_S, the thermal gradient, the furnace translation rate, the degree of supersaturation and the measured residual gas pressure (at room temperature) for each growth run (<1K)

References

1. M. Hovinen, J. Ding, A. Salokatve, A.V. Nurmikko, G.C. Hua, D.C. Grillo, J.Han Li He, M. Ringle and R.L. Gunshor. J. Appl. Phys. 77 (1995), p. 4150. Abstract-Compendex | Abstract-INSPEC   | Full Text via CrossRef

2. L.H. Kuo, L. Salamanca-Riba, B.J. Wu, G.M. Haugen, J.M. DePuydt, G. Hofler and H. Cheng. J. Vac. Sci. Technol. B 13 (1995), p. 1694. Abstract-Compendex | Abstract-INSPEC   | Full Text via CrossRef

3. C.C. Chu, T.B. Ng, J. Han, G.C. Hua, R.L. Gunshor, E. Ho, E.L. Warlick, L.A. Kolodziejski and A.V. Nurmikko. Appl. Phys. Lett. 69 (1996), p. 602. Abstract-Compendex | Abstract-INSPEC   | OJPS full text | Full Text via CrossRef

4. Z. Yu, D.B. Eason, J. Ren, W.C. Hughes, W.H. Rowland, Jr., J.W. Cook, Jr., J.F. Schetzina, G. Cantwell and W.C. Harsch. J. Vac. Sci. Technol. B 13 (1995), p. 711. Abstract-Compendex | Abstract-INSPEC   | Full Text via CrossRef

5. D. Eason, J. Ren, Z. Yu, C. Hughes, J.W. Cook, Jr., J.F. Schetzina, N.A. El-Masry, G. Cantwell and W.C. Harsch. J. Crystal Growth 150 (1995), p. 718. Abstract | Abstract + References | PDF (628 K)

6. D.B. Eason, Z. Yu, W.C. Hughes, C. Boney, J.W. Cook, Jr., J.F. Schetzina, D.R. Black, G. Cantwell and W.C. Harsch. J. Vac. Sci. Technol. B 13 (1995), p. 1566. Abstract-Compendex | Abstract-INSPEC   | Full Text via CrossRef

7. C. Boney, Z. Yu, W.H. Rowland, Jr., W.C. Hughes, J.W. Cook, Jr., J.F. Schetzina, G. Cantwell and W.C. Harsch. J. Vac. Sci. Technol. B 14(1996), p. 2259. Abstract-INSPEC   | OJPS full text | Full Text via CrossRef

8. H. Wenisch, M. Fehrer, K. Ohkawa, D. Hommel, M. Prokesch, U. Rinas and H. Hartmann. J. Appl. Phys. 82 (1997), p. 4690. Abstract-INSPEC   | OJPS full text | Full Text via CrossRef

9. K.F. Burr and J. Woods. J. Crystal Growth 9 (1971), p. 183. Abstract

10. J.R. Cutter, G.J. Russell and J. Woods. J. Crystal Growth 32 (1976), p. 179. Abstract

11. J.R. Cutter and J. Woods. J. Crystal Growth 47 (1979), p. 405. Abstract

12. H.-Y. Cheng and E. Anderson. J. Crystal Growth 96 (1989), p. 756. Abstract

13. G. Cantwell, W.C. Harsch, H.L. Cotal, B.G. Markey, S.W.S. McKeever and J.E. Thomas. J. Appl. Phys. 71 (1992), p. 2931. Abstract-INSPEC   | Full Text via CrossRef

14. F. Allegretti, A. Carrara and S. Pizzini. J. Crystal Growth 128 (1993), p. 646. Abstract-Compendex | Abstract-INSPEC  

15. H. Hartmann and D. Siche. J. Crystal Growth 138 (1994), p. 260. Abstract

16. C.-H. Su, Proceedings of the SPIE, The International Society for Optical Engineering Vol. 3123, 1997, p. 7.

17. H. Lee, T.S. Kim, T.S. Jeong, H.G. An, J.Y. Kim, C.J. Youn, P.Y. Yu, K.J. Hong, H.J. Lee and Y.J. Shin. J. Crystal Growth 191 (1998), p. 59. SummaryPlus | Full Text + Links | PDF (363 K)

18. E.V. Markov and A.A. Davydov. Izv. Akad. Nauk SSSR Neorgan. Mater. 7 (1971), p. 575.

19. K. Grasza. J. Crystal Growth 146 (1995), p. 65. Abstract | Abstract + References | PDF (381 K)

20. Z. Golacki, Z. Furmanik, M. Gorska, A. Szczerbakow and W. Zahorowski. J. Crystal Growth 60 (1982), p. 150. Abstract

21. Z. Golacki, M. Gorska, T. Warminski and A. Szczerbakow. J. Crystal Growth 74 (1986), p. 129. Abstract

22. W. Palosz, K. Grasza, D. Gillies and G. Jerman. J. Crystal Growth 169 (1996), p. 20. Abstract | Abstract + References | PDF (686 K)

23. C.-H. Su, W. Palosz, S. Feth and S.L. Lehoczky. J. Crystal Growth 192 (1998), p. 386. SummaryPlus | Full Text + Links | PDF (321 K)

24. C.-H. Su, S.L. Lehoczky and F.R. Szofran. J. Crystal Growth 101 (1990), p. 221. Abstract

25. C.-H. Su, M.P. Volz, D.C. Gillies, F.R. Szofran, S.L. Lehoczky, M. Dudley, G.D. Yao and W. Zhou. J. Crystal Growth 128 (1993), p. 627. Abstract-INSPEC | Abstract-Compendex  

26. W. Palosz, F.R. Szofran and S.L. Lehoczky. J. Crystal Growth 142 (1994), p. 215. Abstract

27. C-H. Su, M. Dudley, R. Matyi, S. Feth and S.L. Lehoczky. J. Crystal Growth 208 (2000), p. 237. SummaryPlus | Full Text + Links | PDF (901 K)

28. M.M. Faktor and I. Garrett. Growth of Crystals from the Vapour, Chapman & Hall, London (1974).

29. Y.-G. Sha, C.-H. Su, W. Palosz, M.P. Volz, D.C. Gillies, F.R. Szofran, S.L. Lehoczky, H.-C. Liu and R.F. Brebrick. J. Crystal Growth 146 (1995), p. 42. Abstract | Abstract + References | PDF (518 K)

30. C.-H. Su, Y.-G. Sha, K. Mazuruk, S.L. Lehoczky, H.-C. Liu, R. Fang and R.F. Brebrick. J. Crystal Growth 166 (1996), p. 736. SummaryPlus | Full Text + Links | PDF (589 K)

31. R.F. Brebrick and H.-C. Liu. High Temp. Mater. Sci. 35 (1996), p. 215. Abstract-INSPEC  

32. N. Ramachandran, C-H. Su and S.L. Lehoczky. J. Crystal Growth 208 (2000), p. 269. Abstract | PDF (543 K)

33. A. Worlikar, M. R. Overholt, S. Motakef, C-H. Su, N. Ramachandran, Presented at the 11th American Conference on Crystal Growth and Epitaxy (ACCGE-11), Tucson, Arizona, August 1–6, 1999.

34. C.-H. Su, S. Feth, S. L. Lehoczky, J. Crystal Growth 209 (2000) 681.

¹ Universities Space Research Association.

² University of Alabama in Huntsville.

Corresponding author. Tel.: +1-256-544-7776; fax: +1-256-5448762; email: ching.hua.su@msfc.nasa.gov