Abstract

We used two-dimensional laser Raman scattering and elastic light scattering to analyze mixture driven particle formation in the supercritical antisolvent process. Using only one excitation laser, the partial density of the antisolvent CO2, the composition of the solvent/antisolvent mixture, and the occurrence of particle formation can be analyzed simultaneously. Thus, all main parameters that influence the process of particle formation and, sub sequently, the desired properties of the produced powder are accessible.

© 2010 Optical Society of America

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  1. C. A. Eckert, B. L. Knutson, and P. G. Debenedetti, Nature 383, 313 (1996).
    [CrossRef]
  2. B. Y. Shekunov and P. York, J. Cryst. Growth 211, 122 (2000).
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    [CrossRef]
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    [CrossRef] [PubMed]
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    [CrossRef]
  9. E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
    [CrossRef]
  10. A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
    [CrossRef]

2010

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

2009

A. Braeuer, S. R. Engel, R. F. Hankel, and A. Leipertz, Opt. Lett. 34, 3122 (2009).
[CrossRef] [PubMed]

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

2007

A. E. Andreatta, L. J. Florusse, S. B. Bottini, and C. J. Peters, J. Supercrit. Fluids 42, 60 (2007).
[CrossRef]

2002

2000

B. Y. Shekunov and P. York, J. Cryst. Growth 211, 122 (2000).
[CrossRef]

1996

C. A. Eckert, B. L. Knutson, and P. G. Debenedetti, Nature 383, 313 (1996).
[CrossRef]

1995

A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
[CrossRef]

Andreatta, A. E.

A. E. Andreatta, L. J. Florusse, S. B. Bottini, and C. J. Peters, J. Supercrit. Fluids 42, 60 (2007).
[CrossRef]

Bottini, S. B.

A. E. Andreatta, L. J. Florusse, S. B. Bottini, and C. J. Peters, J. Supercrit. Fluids 42, 60 (2007).
[CrossRef]

Braeuer, A.

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

A. Braeuer, S. R. Engel, R. F. Hankel, and A. Leipertz, Opt. Lett. 34, 3122 (2009).
[CrossRef] [PubMed]

Debenedetti, P. G.

C. A. Eckert, B. L. Knutson, and P. G. Debenedetti, Nature 383, 313 (1996).
[CrossRef]

Dowy, S.

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

Eckert, C. A.

C. A. Eckert, B. L. Knutson, and P. G. Debenedetti, Nature 383, 313 (1996).
[CrossRef]

Engel, S. R.

Florusse, L. J.

A. E. Andreatta, L. J. Florusse, S. B. Bottini, and C. J. Peters, J. Supercrit. Fluids 42, 60 (2007).
[CrossRef]

Hankel, R. F.

Hartley, D. L.

D. L. Hartley, in Laser Raman Gas Diagnostics, M.Lapp and C.M.Penney, eds. (Plenum, 1974), pp. 1151–1157.

Knutson, B. L.

C. A. Eckert, B. L. Knutson, and P. G. Debenedetti, Nature 383, 313 (1996).
[CrossRef]

Kojima, J.

Kordikowski, A.

A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
[CrossRef]

Leipertz, A.

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

A. Braeuer, S. R. Engel, R. F. Hankel, and A. Leipertz, Opt. Lett. 34, 3122 (2009).
[CrossRef] [PubMed]

Long, D. A.

D. A. Long, Raman Spectroscopy (McGraw-Hill, 1977).

Nguyen, Q.-V.

Peters, C. J.

A. E. Andreatta, L. J. Florusse, S. B. Bottini, and C. J. Peters, J. Supercrit. Fluids 42, 60 (2007).
[CrossRef]

A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
[CrossRef]

Reverchon, E.

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

Schatz, R.

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

Schenk, A. P.

A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
[CrossRef]

Schluecker, E.

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

Shekunov, B. Y.

B. Y. Shekunov and P. York, J. Cryst. Growth 211, 122 (2000).
[CrossRef]

Torino, E.

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

Van Nielen, R. M.

A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
[CrossRef]

York, P.

B. Y. Shekunov and P. York, J. Cryst. Growth 211, 122 (2000).
[CrossRef]

Appl. Opt.

Chem. Eng. J.

E. Reverchon, E. Torino, S. Dowy, A. Braeuer, and A. Leipertz, Chem. Eng. J. 156, 446 (2010).
[CrossRef]

J. Cryst. Growth

B. Y. Shekunov and P. York, J. Cryst. Growth 211, 122 (2000).
[CrossRef]

J. Supercrit. Fluids

S. Dowy, A. Braeuer, R. Schatz, E. Schluecker, and A. Leipertz, J. Supercrit. Fluids 48, 195 (2009).
[CrossRef]

A. Kordikowski, A. P. Schenk, R. M. Van Nielen, and C. J. Peters, J. Supercrit. Fluids 8, 205 (1995).
[CrossRef]

A. E. Andreatta, L. J. Florusse, S. B. Bottini, and C. J. Peters, J. Supercrit. Fluids 42, 60 (2007).
[CrossRef]

Nature

C. A. Eckert, B. L. Knutson, and P. G. Debenedetti, Nature 383, 313 (1996).
[CrossRef]

Opt. Lett.

Other

D. L. Hartley, in Laser Raman Gas Diagnostics, M.Lapp and C.M.Penney, eds. (Plenum, 1974), pp. 1151–1157.

D. A. Long, Raman Spectroscopy (McGraw-Hill, 1977).

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Figures (3)

Fig. 1
Fig. 1

Schematic of the Raman scattering and elastic light scattering setup: M, mirror; BS, beam splitter; SL, spherical lens; CL, cylindrical lens; BD, beam dump; OL, objective lens; DM, dichroic mirror; BPF, bandpass filter; LPF, long-pass filter; and EMCCD-C, electron-multiplying CCD camera.

Fig. 2
Fig. 2

Simultaneously acquired single-shot images of (a) the CO 2 mole fraction x CO 2 , (b) the CO 2 partial density distribution ρ CO 2 , and (c) the phase boundary distribution indicating particle formation at a chamber pressure of 16 MPa ( CO 2 flow rate 53 g min 1 ) and an injection flow rate of 2.2 g min 1 at 313 K .

Fig. 3
Fig. 3

Mean images of (a) the CO 2 mole fraction x CO 2 , (b) the CO 2 partial density distribution ρ CO 2 , and (c) the phase boundary distribution indicating particle formation at a chamber pressure of 16 MPa ( CO 2 flow rate 53 g min 1 ) and an injection flow rate of 2.2 g min 1 at 313 K . Left column, injection of pure DMSO into CO 2 . Right column, injection of a YAc/DMSO ( 1 wt . % ) solution into CO 2 .

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