Abstract
The scarcity of high-resolution, in situ tools has left many fundamental questions regarding crystallization processes unanswered. Recent years have seen many advances in transmission electron microscopy (TEM) approaches that allow TEM observations of liquid environments. These liquid phase TEM techniques provide an in situ platform for investigating the early events in materials formation and understanding the mechanisms by which crystals develop. In this chapter, we provide an overview of the liquid phase TEM experimental platforms and discuss recent studies that use the technique to address open questions in crystallization. We first highlight liquid phase TEM investigations into the calcium carbonate system, where the technique provides insights into the formation pathways that take the mineral from its solvated state to one of various solid phases and the effect that an organic additive can have on such processes. In the following section, we discuss studies of metal nanoparticle formation that investigate the mechanisms of nucleation and growth from a precursor solution, as well as the development into faceted nanocrystals in the presence of an organic ligand. We close the chapter with a discussion of areas for future development that would broaden the utility of liquid phase TEM.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Addadi L, Moradian J, Shay E, Maroudas NG, Weiner S (1987) A chemical model for the cooperation of sulfates and carboxylates in calcite crystal nucleation: relevance to biomineralization. Proc Natl Acad Sci U S A 84(9):2732–2736. doi:10.1073/pnas.84.9.2732
Ando T, Kodera N, Takai E, Maruyama D, Saito K, Toda A (2001) A high-speed atomic force microscope for studying biological macromolecules. Proc Natl Acad Sci 98(22):12468–12472. doi:10.1073/pnas.211400898
Andreassen JP, Beck R, Nergaard M (2012) Biomimetic type morphologies of calcium carbonate grown in absence of additives. Faraday Discuss 159:247–261. doi:10.1039/c2fd20056b
Baumgartner J, Dey A, Bomans PHH, Le Coadou C, Fratzl P, Sommerdijk N, Faivre D (2013) Nucleation and growth of magnetite from solution. Nat Mater 12(4):310–314. doi:10.1038/nmat3558
Bewernitz MA, Gebauer D, Long J, Cölfen H, Gower LB (2012) A metastable liquid precursor phase of calcium carbonate and its interactions with polyaspartate. Faraday Discuss 159:291–312. doi:10.1039/c2fd20080e
Bots P, Benning LG, Rodriguez-Blanco JD, Roncal-Herrero T, Shaw S (2012) Mechanistic insights into the crystallization of Amorphous Calcium Carbonate (ACC). Cryst Growth Des 12(7):3806–3814. doi:10.1021/cg300676b
Brecevic L, Nielsen AE (1989) Solubility of amorphous calcium carbonate. J Cryst Growth 98(3):504–510. doi:10.1016/0022-0248(89)90168-1
Birkedal H (2017) Phase transformations in calcium phosphate crystallization. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth: from solution precursors to solid materials. Springer, Cham, pp 199–210
Brooks R, Clark LM, Thurston EF (1950) Calcium carbonate and its hydrates. Philos Trans R Soc London Ser A Math Phys Sci 243(861):145–167. doi:10.1098/rsta.1950.0016
Cardew PT, Davey RJ (1985) The kinetics of solvent-mediated phase transformations. Proc R Soc London Ser A-Math Phys Eng Sci 398(1815):415–428
Chernov AA (1984) Modern crystallography III, vol 36, Springer series in solid-state sciences. Springer, Berlin
De Yoreo JJ, Sommerdijk NAJM, Dove PM (2017) Nucleation pathways in electrolyte solutions. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 1–24
Delgado-López JM, Guagliardi A (2017) Control over nanocrystalline apatite formation: what can the X-ray total scattering approach tell us. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 211–226
Demichelis R, Raiteri P, Gale JD, Quigley D, Gebauer D (2011) Stable prenucleation mineral clusters are liquid-like ionic polymers. Nat Commun 2:590. doi:10.1038/ncomms1604
Evans JE, Jungjohann KL, Wong PCK, Chiu P-L, Dutrow GH, Arslan I, Browning ND (2012) Visualizing macromolecular complexes with In Situ liquid scanning transmission electron microscopy. Micron 43(11):1085–1090. doi:10.1016/j.micron.2012.01.018
Falini G, Fermani S (2017) Nucleation and growth from a biomineralization perspective. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 185–198
Fang PA, Conway JF, Margolis HC, Simmer JP, Beniash E (2011) Hierarchical self-assembly of amelogenin and the regulation of biomineralization at the nanoscale. Proc Natl Acad Sci U S A 108(34):14097–14102. doi:10.1073/pnas.1106228108
Fernandez-Martinez A, Lopez-Martinez H, Wang D (2017) Structural characteristics and the occurrence of polyamorphism in amorphous calcium carbonate. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 77–92
Frandsen C, Legg BA, Comolli LR, Zhang HZ, Gilbert B, Johnson E, Banfield JF (2014) Aggregation-induced growth and transformation of Beta-FeOOH nanorods to micron-sized Alpha-Fe2O3 spindles. CrystEngComm 16(8):1451–1458. doi:10.1039/c3ce40983j
Gal A, Habraken W, Gur D, Fratzl P, Weiner S, Addadi L (2013) Calcite crystal growth by a solid-state transformation of stabilized amorphous calcium carbonate nanospheres in a hydrogel. Angew Chem Int Ed 52(18):4867–4870. doi:10.1002/anie.201210329
Galkin O, Chen K, Nagel RL, Hirsch RE, Vekilov PG (2002) Liquid-liquid separation in solutions of normal and sickle cell hemoglobin. Proc Natl Acad Sci U S A 99(13):8479–8483. doi:10.1073/pnas.122055299
Gebauer D, Völkel A, Cölfen H (2008) Stable prenucleation calcium carbonate clusters. Science 322(5909):1819–1822. doi:10.1126/science.1164271
Gebauer D, Gunawidjaja PN, Ko JYP, Bacsik Z, Aziz B, Liu LJ, Hu YF, Bergström L, Tai CW, Sham TK, Eden M, Hedin N (2010) Proto-calcite and proto-vaterite in amorphous calcium carbonates. Angew Chem-Int Ed 49(47):8889–8891. doi:10.1002/anie.201003220
Gehrke N, Cölfen H, Pinna N, Antonietti M, Nassif N (2005) Superstructure of calcium carbonate crystals by oriented attachment. Cryst Growth Des 5(4):1317–1319. doi:10.1021/cg050051d
Gibbs JW (1876) On the equilibrium of heterogeneous substances. Trans Connecticut Acad Arts Sci 3:108–248
Gibbs JW (1878) On the equilibrium of heterogeneous substances. Trans Connecticut Acad Arts Sci 3:343–524
Giuffre AJ, Hamm LM, Han N, De Yoreo JJ, Dove PM (2013) Polysaccharide chemistry regulates kinetics of calcite nucleation through competition of interfacial energies. Proc Natl Acad Sci 110(23):9261–9266. doi:10.1073/pnas.1222162110
Grogan JM, Bau HH (2010) The nanoaquarium: a platform for In Situ transmission electron microscopy in liquid media. J Microelectromech Syst 19(4):885–894. doi:10.1109/jmems.2010.2051321
Grogan JM, Schneider NM, Ross FM, Bau HH (2014) Bubble and pattern formation in liquid induced by an electron beam. Nano Lett 14(1):359–364. doi:10.1021/nl404169a
Habraken W, Tao JH, Brylka LJ, Friedrich H, Bertinetti L, Schenk AS, Verch A, Dmitrovic V, Bomans PHH, Frederik PM, Laven J, van der Schoot P, Aichmayer B, de With G, DeYoreo JJ, Sommerdijk N (2013) Ion-association complexes unite classical and Non-classical theories for the biomimetic nucleation of calcium phosphate. Nat Commun 4:1507. doi:10.1038/ncomms2490
Hamm LM, Giuffre AJ, Han N, Tao J, Wang D, De Yoreo JJ, Dove PM (2014) Reconciling disparate views of template-directed nucleation through measurement of calcite nucleation kinetics and binding energies. Proc Natl Acad Sci 111(4):1304–1309. doi:10.1073/pnas.1312369111
Hu Q, Nielsen MH, Freeman CL, Hamm LM, Tao J, Lee JRI, Han TYJ, Becker U, Harding JH, Dove PM, De Yoreo JJ (2012) The thermodynamics of calcite nucleation at organic interfaces: classical vs. Non-classical pathways. Faraday Discuss 159:509–523. doi:10.1039/c2fd20124k
Johnston J, Merwin HE, Williamson ED (1916) The several forms of calcium carbonate. Am J Sci 41(246):473–512
Koga N, Yamane Y (2008) Thermal behaviors of amorphous calcium carbonates prepared in aqueous and ethanol media. J Therm Anal Calorim 94(2):379–387. doi:10.1007/s10973-008-9110-3
Krauss F, Schriever W (1930) The hydrates of calcium carbonate. Zeitschrift Fur Anorganische Und Allgemeine Chemie 188(1):259–260. doi:10.1002/zaac.19301880122
Lee JRI, Han TYJ, Willey TM, Wang D, Meulenberg RW, Nilsson J, Dove PM, Terminello LJ, van Buuren T, De Yoreo JJ (2007) Structural development of mercaptophenol self-assembled monolayers and the overlying mineral phase during templated CaCO3 crystallization from a transient amorphous film. J Am Chem Soc 129(34):10370–10381. doi:10.1021/ja071535w
Li DS, Nielsen MH, Lee JRI, Frandsen C, Banfield JF, De Yoreo JJ (2012) Direction-specific interactions control crystal growth by oriented attachment. Science 336(6084):1014–1018. doi:10.1126/science.1219643
Liao H-G, Zherebetskyy D, Xin H, Czarnik C, Ercius P, Elmlund H, Pan M, Wang L-W, Zheng H (2014) Facet development during platinum nanocube growth. Science 345(6199):916–919. doi:10.1126/science.1253149
Lifshitz IM, Slyozov VV (1961) The kinetics of precipitation from supersaturated solid solutions. J Phys Chem Solids 19(1–2):35–50. doi:10.1016/0022-3697(61)90054-3
Mann S (1993) Molecular tectonics in biomineralization and biomimetic materials chemistry. Nature 365(6446):499–505. doi:10.1038/365499a0
Marsh ME (1994) Polyanion-mediated mineralization – assembly and reorganization of acidic polysaccharides in the Golgi system of a coccolithophorid alga during mineral deposition. Protoplasma 177(3–4):108–122. doi:10.1007/bf01378985
Nielsen MH, De Yoreo JJ (2016) Liquid cell TEM for studying environmental and biological mineral systems. In: Ross FM (ed) Liquid cell electron microscopy. Cambridge University Press, Cambridge
Nielsen MH, Lee JRI, Hu QN, Han TYJ, De Yoreo JJ (2012) Structural evolution, formation pathways and energetic controls during template-directed nucleation of CaCO3. Faraday Discuss 159:105–121. doi:10.1039/c2fd20050c
Nielsen MH, Li DS, Zhang HZ, Aloni S, Han TYJ, Frandsen C, Seto J, Banfield JF, Cölfen H, De Yoreo JJ (2014a) Investigating processes of nanocrystal formation and transformation via liquid cell TEM. Microsc Microanal 20(2):425–436. doi:10.1017/s1431927614000294
Nielsen MH, Aloni S, De Yoreo JJ (2014b) In Situ TEM imaging of CaCO3 nucleation reveals coexistence of direct and indirect pathways. Science 345(6201):1158–1162. doi:10.1126/science.1254051
Nudelman F, Gotliv BA, Addadi L, Weiner S (2006) Mollusk shell formation: mapping the distribution of organic matrix components underlying a single aragonitic tablet in nacre. J Struct Biol 153(2):176–187. doi:10.1016/j.jsb.2005.09.009
Nudelman F, Pieterse K, George A, Bomans PHH, Friedrich H, Brylka LJ, Hilbers PAJ, de With G, Sommerdijk N (2010) The role of collagen in bone apatite formation in the presence of hydroxyapatite nucleation inhibitors. Nat Mater 9(12):1004–1009. doi:10.1038/nmat2875
Penn RL (2004) Kinetics of oriented aggregation. J Phys Chem B 108(34):12707–12712. doi:10.1021/jp036490+
Penn RL, Banfield JF (1998a) Oriented attachment and growth, twinning, polytypism, and formation of metastable phases: insights from nanocrystalline TiO2. Am Mineral 83(9–10):1077–1082
Penn RL, Banfield JF (1998b) Imperfect oriented attachment: dislocation generation in defect-free nanocrystals. Science 281(5379):969–971. doi:10.1126/science.281.5379.969
Penn RL, Li D, Soltis JA (2017) A perspective on the particle-based crystal growth of ferric oxides, oxyhydroxides, and hydrous oxides. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 257–274
Pouget EM, Bomans PHH, Goos JACM, Frederik PM, de With G, Sommerdijk NAJM (2009) The initial stages of template-controlled CaCO3 formation revealed by Cryo-TEM. Science 323(5920):1555–1458. doi:10.1126/science.1169434
Radha AV, Forbes TZ, Killian CE, Gilbert P, Navrotsky A (2010) Transformation and crystallization energetics of synthetic and biogenic amorphous calcium carbonate. Proc Natl Acad Sci U S A 107(38):16438–16443. doi:10.1073/pnas.1009959107
Rao A, Cölfen H (2017) Mineralization schemes in the living world: mesocrystals. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 155–184
Reichel V, Faivre D (2017) Magnetite nucleation and growth. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 275–292
Rieger J, Thieme J, Schmidt C (2000) Study of precipitation reactions by X-ray microscopy: CaCO3 precipitation and the effect of polycarboxylates. Langmuir 16(22):8300–8305. doi:10.1021/la0004193
Rieger J, Frechen T, Cox G, Heckmann W, Schmidt C, Thieme J (2007) Precursor structures in the crystallization/precipitation processes of CaCO3 and control of particle formation by polyelectrolytes. Faraday Discuss 136:265–277. doi:10.1039/b701450c
Ring EA, de Jonge N (2010) Microfluidic system for transmission electron microscopy. Microsc Microanal 16(5):622–629. doi:10.1017/s1431927610093669
Rodriguez-Blanco JG, Sand KK, Benning LG (2017) ACC and vaterite as intermediates in the solution-based crystallization of CaCO3. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 93–112
Schneider NM, Norton MM, Mendel BJ, Grogan JM, Ross FM, Bau HH (2014) Electron-water interactions and implications for liquid cell electron microscopy. J Phys Chem C 118(38):22373–22382. doi:10.1021/jp507400n
Sleutel M, Lutsko J, Van Driessche AES, Duran-Olivencia MA, Maes D (2014) Observing classical nucleation theory at work by monitoring phase transitions with molecular precision. Nat Commun 5:5598. doi:10.1038/ncomms6598
Smeets PJM, Cho KR, Kempen RGE, Sommerdijk NAJM, De Yoreo JJ (2015) Calcium carbonate nucleation driven by Ion binding in a biomimetic matrix revealed by in situ electron microscopy. Nat Mater 14:394–399. doi:10.1038/nmat4193
Tester CC, Brock RE, Wu CH, Krejci MR, Weigand S, Joester D (2011) In Vitro synthesis and stabilization of Amorphous Calcium Carbonate (ACC) nanoparticles within liposomes. CrystEngComm 13(12):3975–3978. doi:10.1039/c1ce05153a
Trotsenko O, Roiter Y, Minko S (2012) Conformational transitions of flexible hydrophobic polyelectrolytes in solutions of monovalent and multivalent salts and their mixtures. Langmuir 28(14):6037–6044. doi:10.1021/la300584k
Verch A, Morrison IEG, van de Locht R, Kroger R (2013) In Situ electron microscopy studies of calcium carbonate precipitation from aqueous solution with and without organic additives. J Struct Biol 183(2):270–277. doi:10.1016/j.jsb.2013.05.017
Voorhees PW (1985) The theory of Ostwald ripening. J Stat Phys 38(1–2):231–252. doi:10.1007/bf01017860
Wagner C (1961) Theorie der Alterung von Niederschlagen durch Umlosen (Ostwald-Reifung). Z Elektrochem 65(7–8):581–591
Wallace AF, Hedges LO, Fernandez-Martinez A, Raiteri P, Gale JD, Waychunas GA, Whitelam S, Banfield JF, De Yoreo JJ (2013) Microscopic evidence for liquid-liquid separation in supersaturated CaCO3 solutions. Science 341(6148):885–889. doi:10.1126/science.1230915
Williamson MJ, Tromp RM, Vereecken PM, Hull R, Ross FM (2003) Dynamic microscopy of nanoscale cluster growth at the solid-liquid interface. Nat Mater 2(8):532–536. doi:10.1038/nmat944
Woehl TJ, Evans JE, Arslan L, Ristenpart WD, Browning ND (2012) Direct in Situ determination of the mechanisms controlling nanoparticle nucleation and growth. ACS Nano 6(10):8599–8610. doi:10.1021/nn303371y
Woehl TJ, Jungjohann KL, Evans JE, Arslan I, Ristenpart WD, Browning ND (2013) Experimental procedures to mitigate electron beam induced artifacts during In Situ fluid imaging of nanomaterials. Ultramicroscopy 127:53–63. doi:10.1016/j.ultramic.2012.07.018
Wolf SE, Gower LB (2017) Challenges and perspectives of the polymer-induced liquid-precursor process: the pathway from liquid-condensed mineral precursors to mesocrystalline products. In: Van Driessche AES, Kellermeier M, Benning LG, Gebauer D (eds) New perspectives on mineral nucleation and growth, Springer, Cham, pp 43–76
Wulff G (1901) On the question of speed of growth and dissolution of crystal surfaces. Zeitschrift für Krystallographie und Mineralogie 34(5/6):449–530
Yin Y, Alivisatos AP (2005) Colloidal nanocrystal synthesis and the organic-inorganic interface. Nature 437(7059):664–670. doi:10.1038/nature04165
Yuk JM, Park J, Ercius P, Kim K, Hellebusch DJ, Crommie MF, Lee JY, Zettl A, Alivisatos AP (2012) High-resolution EM of colloidal nanocrystal growth using graphene liquid cells. Science 336(6077):61–64. doi:10.1126/science.1217654
Zheng HM, Smith RK, Jun YW, Kisielowski C, Dahmen U, Alivisatos AP (2009) Observation of single colloidal platinum nanocrystal growth trajectories. Science 324(5932):1309–1312. doi:10.1126/science.1172104
Acknowledgments
The authors acknowledge support from the National Science Foundation under grant DMR-1312697. Additional support for this work was provided by the Laboratory Directed Research and Development Initiative on Materials Synthesis and Simulation Across Scales at the Pacific Northwest National Laboratory (PNNL). PNNL is operated by Battelle for the US Department of Energy under Contract DE-AC05-76RL01830. Work conducted at LLNL was performed under the auspices of the US DOE by LLNL under Contract DE-AC52-07NA20344.
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2017 Springer International Publishing Switzerland
About this chapter
Cite this chapter
Nielsen, M.H., De Yoreo, J.J. (2017). Liquid Phase TEM Investigations of Crystal Nucleation, Growth, and Transformation. In: Van Driessche, A., Kellermeier, M., Benning, L., Gebauer, D. (eds) New Perspectives on Mineral Nucleation and Growth. Springer, Cham. https://doi.org/10.1007/978-3-319-45669-0_18
Download citation
DOI: https://doi.org/10.1007/978-3-319-45669-0_18
Published:
Publisher Name: Springer, Cham
Print ISBN: 978-3-319-45667-6
Online ISBN: 978-3-319-45669-0
eBook Packages: Earth and Environmental ScienceEarth and Environmental Science (R0)