Crystal shape distribution, i.e. the multidimensional size distribution of crystals, is of great importance to their down-stream processing such as in filtration as well as to the end-use properties including the dissolution rate and bioavailability for crystalline pharmaceuticals. Engineering crystal shape and shape distribution requires knowledge about the growth behavior of different crystal facets under varied operational conditions e.g. supersaturations. Measurement of the facet growth rates and growth kinetics of static crystals in a crystallizer without stirring has been reported previously. Here attention is given to study on real-time characterization of the 3D facet growth behavior of crystals in a stirred tank where crystals are constantly moving and rotating. The measurement technique is stereo imaging and the crystal shape reconstruction is based on a stereo imaging camera model. By reference to a case study on potash alum crystallization, it is demonstrated that the crystal size and shape distributions (CSSD) of moving and rotating potash alum crystals in the solution can be reconstructed. The moving window approach was used to correlate 3D face growth kinetics with supersaturation (in the range 0.04 - 0.12) given by an ATR FTIR probe. It revealed that {100} is the fastest growing face, leading to a rapid reduction of its area, while the {111} face has the slowest growth rate, reflected in its area continuously getting larger.
References
[1]
Zhang, R., Ma, C.Y., Liu, J.J. and Wang, X.Z. (2015) On-Line Measurement of the Real Size and Shape of Crystals in Stirred Tank Crystalliser Using Non-Invasive Stereo Vision Imaging. Chemical Engineering Science, 137, 9-21.
https://doi.org/10.1016/j.ces.2015.05.053
[2]
Wu, K., Ma, C.Y., Liu, J.J., Zhang, Y. and Wang, X.Z. (2016) Measurement of Crystal Face Specific Growth Kinetics. Crystal Growth & Design, 16, 4855-4868.
https://doi.org/10.1021/acs.cgd.6b00189
[3]
Ma, C.Y., Liu, J.J. and Wang, X.Z. (2016) Stereo Imaging of Crystal Growth. AIChE Journal, 62, 18-25. https://doi.org/10.1002/aic.15041
[4]
Zhang, R., Ma, C.Y., Liu, J.J., Zhang, Y., Liu, Y.J. and Wang, X.Z. (2017) Stereo Imaging Camera Model for 3D Shape Reconstruction of Complex Crystals and Estimation of Facet Growth Kinetics. Chemical Engineering Science, 160, 171-182.
https://doi.org/10.1016/j.ces.2016.11.029
[5]
Ma, C.Y., Liu, J.J. and Wang, X.Z. (2016) Measurement, Modelling, and Closed-Loop Control of Crystal Shape Distribution: Literature Review and Future Perspectives. Particuology, 26, 1-18. https://doi.org/10.1016/j.partic.2015.09.014
[6]
Wang, X.Z., Roberts, K.J. and Ma, C. (2008) Crystal Growth Measurement Using 2D and 3D Imaging and the Perspectives for Shape Control. Chemical Engineering Science, 63, 1173-1184. https://doi.org/10.1016/j.ces.2007.07.018
[7]
Zhang, Y., Liu, J.J., Zhang, L., De Anda, J.C. and Wang, X.Z. (2016) Particle Shape Characterisation and Classification Using Automated Microscopy and Shape Descriptors in Batch Manufacture of Particulate Solids. Particuology, 24, 61-68.
https://doi.org/10.1016/j.partic.2014.12.012
[8]
Li, R.F., Thomson, G.B., White, G., Wang, X.Z., De Anda, J.C. and Roberts, K.J. (2006) Integration of Crystal Morphology Modeling and On-Line Shape Measurement. AIChE Journal, 52, 2297-2305. https://doi.org/10.1002/aic.10818
[9]
Borchert, C., Temmel, E., Eisenschmidt, H., Lorenz, H., Seidel-Morgenstern, A. and Sundmacher, K. (2014) Image-Based in Situ Identification of Face Specific Crystal Growth Rates from Crystal Populations. Crystal Growth & Design, 14, 952-971.
https://doi.org/10.1021/cg401098x
[10]
Kempkes, M., Vetter, T. and Mazzotti, M. (2010) Measurement of 3D Particle Size Distributions by Stereoscopic Imaging. Chemical Engineering Science, 65, 1362-1373.
https://doi.org/10.1016/j.ces.2009.10.008
[11]
Schorsch, S., Vetter, T. and Mazzotti, M. (2012) Measuring Multidimensional Particle Size Distributions during Crystallization. Chemical Engineering Science, 77, 130-142. https://doi.org/10.1016/j.ces.2011.11.029
[12]
Schorsch, S., Ochsenbein, D.R., Vetter, T., Morari, M. and Mazzotti, M. (2014) High Accuracy Online Measurement of Multidimensional Particle Size Distributions during Crystallization. Chemical Engineering Science, 105, 155-168.
https://doi.org/10.1016/j.ces.2013.11.003
[13]
Schorsch, S., Hours, J.-H., Vetter, T., Mazzotti, M. and Jones, C.N. (2015) An Optimization-Based Approach to Extract Faceted Crystal Shapes from Stereoscopic Images. Computers & Chemical Engineering, 75, 171-183.
https://doi.org/10.1016/j.compchemeng.2015.01.016
[14]
Huo, Y., Liu, T., Liu, H., Ma, C.Y. and Wang, X.Z. (2016) In-Situ Crystal Morphology Identification Using Imaging Analysis with Application to the L-Glutamic Acid Crystallization. Chemical Engineering Science, 148, 126-139.
https://doi.org/10.1016/j.ces.2016.03.039
[15]
Huo, Y., Liu, T., Wang, X.Z., Ma, C.Y. and Ni, X. (2017) Online Detection of Particle Agglomeration during Solution Crystallization by Microscopic Double-View Image Analysis. Industrial & Engineering Chemistry Research, 56, 11257-11269.
https://doi.org/10.1021/acs.iecr.7b02439
[16]
Kovačević, T., Reinhold, A. and Briesen, H. (2014) Identifying Faceted Crystal Shape from Three-Dimensional Tomography Data. Crystal Growth & Design, 14, 1666-1675. https://doi.org/10.1021/cg401780p
[17]
Kovačević, T., Schock, J., Pfeiffer, F. and Briesen, H. (2016) Shape Identification of Primary Particles in Potash Alum Aggregates Using Three-Dimensional Tomography Data. Crystal Growth & Design, 16, 2685-2699.
https://doi.org/10.1021/acs.cgd.5b01806
[18]
Kovačević, T., Wiedmeyer, V., Schock, J., Voigt, A., Pfeiffer, F., Sundmacher, K. and Briesen, H. (2017) Disorientation Angle Distribution of Primary Particles in Potash Alum Aggregates. Journal of Crystal Growth, 467, 93-106.
https://doi.org/10.1016/j.jcrysgro.2017.03.026
[19]
Indhumathi, C., Cai, Y.Y., Guan, Y.Q. and Opas, M. (2011) An Automatic Segmentation Algorithm for 3D Cell Cluster Splitting Using Volumetric Confocal Images. Journal of Microscopy, 243, 60. https://doi.org/10.1111/j.1365-2818.2010.03482.x
[20]
Singh, M.R., Chakraborty, J., Nere, N., Tung, H.H., Bordawekar, S. and Ramkrishna, D. (2012) Image-Analysis-Based Method for 3D Crystal Morphology Measurement and Polymorph Identification Using Confocal Microscopy. Crystal Growth & Design, 12, 3735-3748. https://doi.org/10.1021/cg300547w
[21]
Stock, S. (2009) Micro-Computed Tomography. CRC Press, Taylor & Francis Group, Boca Raton.
[22]
Erdoğan, S.T., Nie, X., Stutzman, P.E. and Garboczi, E.J. (2010) Micrometer-Scale 3-D Shape Characterization of Eight Cements: Particle Shape and Cement Chemistry, and the Effect of Particle Shape on Laser Diffraction Particle Size Measurement. Cement & Concrete Research, 40, 731-739.
https://doi.org/10.1016/j.cemconres.2009.12.006
[23]
Frisullo, P., Barnabà, M., Navarini, L. and Del Nobile, M.A. (2012) Coffea arabica Beans Microstructural Changes Induced by Roasting: An X-Ray Microtomographic Investigation. Journal of Food Engineering, 108, 232-237.
https://doi.org/10.1016/j.jfoodeng.2011.07.036
[24]
Jerram, D.A., Mock, A., Davis, G.R., Field, M. and Brown, R.J. (2009) 3D Crystal Size Distributions: A Case Study on Quantifying Olivine Populations in Kimberlites. Lithos, 112, 223-235. https://doi.org/10.1016/j.lithos.2009.05.042
[25]
Redenbach, C., Ohser-Wiedemann, R., Löffler, R., Bernthaler, T. and Nagel, A. (2011) Characterization of Powders Using Micro Computed Tomography. Particle & Particle Systems Characterization, 28, 3-12.
https://doi.org/10.1002/ppsc.200900088
[26]
Dandekar, P., Kuvadia, Z.B. and Doherty, M.F. (2013) Engineering Crystal Morphology. Annual Review of Materials Research, 43, 359-386.
https://doi.org/10.1146/annurev-matsci-071312-121623
[27]
Klapper, H., Becker, R.A., Schmiemann, D. and Faber, A. (2002) Growth-Sector Boundaries and Growth-Rate Dispersion in Potassium Alum Crystals. Crystal Research and Technology, 37, 747-757.
https://doi.org/10.1002/1521-4079(200207)37:7<747::AID-CRAT747>3.0.CO;2-2
[28]
Ma, C.Y., Wang, X.Z. and Roberts, K.J. (2008) Morphological Population Balance for Modeling Crystal Growth in Face Directions. AIChE Journal, 54, 209-222.
https://doi.org/10.1002/aic.11365
[29]
Ristic, R.I., Shekunov, B. and Shewood, J.N. (1996) Long and Short Period Growth Rate Variations in Potash Alum Crystals. Journal of Crystal Growth, 160, 330-336.
https://doi.org/10.1016/0022-0248(95)00741-5
[30]
Ristic, R.I., Shekunov, B.Y. and Sherwood, J.N. (1997) The Influence of Synchrotron Radiation-Induced Strain on the Growth and Dissolution of Brittle and Ductile Materials. Journal of Crystal Growth, 179, 205-212.
https://doi.org/10.1016/S0022-0248(97)00106-1
[31]
Barrett, P. and Glennon, B. (2002) Characterizing the Metastable Zone Width and Solubility Curve Using Lasentec FBRM and PVM. Chemical Engineering Research and Design, 80, 799-805. https://doi.org/10.1205/026387602320776876
[32]
Nollet, S., Hilgers, C. and Urai, J.L. (2006) Experimental Study of Polycrystal Growth from an Advecting Supersaturated Fluid in a Model Fracture. Geofluids, 6, 185-200. https://doi.org/10.1111/j.1468-8123.2006.00142.x
[33]
Ma, C.Y. and Wang, X.Z. (2012) Model Identification of Crystal Facet Growth Kinetics in Morphological Population Balance Modeling of L-Glutamic Acid Crystallization and Experimental Validation. Chemical Engineering Science, 70, 22-30.
https://doi.org/10.1016/j.ces.2011.05.042
[34]
Ma, C.Y. and Wang, X.Z. (2012) Closed-Loop Control of Crystal Shape in Cooling Crystallization of L-Glutamic Acid. Journal of Process Control, 22, 72-81.
https://doi.org/10.1016/j.jprocont.2011.10.007
[35]
Wold, S., Sjöström, M. and Eriksson, L. (2001) PLS-Regression: A Basic Tool of Chemometrics. Chemometrics and Intelligent Laboratory Systems, 58, 109-130.
https://doi.org/10.1016/S0169-7439(01)00155-1
[36]
Wan, J., Wang, X.Z. and Ma, C.Y. (2009) Particle Shape Manipulation and Optimization in Cooling Crystallization Involving Multiple Crystal Morphological Forms. AIChE Journal, 55, 2049-2061. https://doi.org/10.1002/aic.11892
[37]
Calderon De Anda, J., Wang, X.Z. and Roberts, K.J. (2005) Multi-Scale Segmentation Image Analysis for the In-Process Monitoring of Particle Shape with Batch Crystallisers. Chemical Engineering Science, 60, 1053-1065.
https://doi.org/10.1016/j.ces.2004.09.068
[38]
Wan, J., Ma, C.Y. and Wang, X.Z. (2008) A Method for Analyzing On-Line Video Images of Crystallization at High-Solid Concentrations. Particuology, 6, 9-15.
https://doi.org/10.1016/j.cpart.2007.11.001
