journal article·2023-02Open access

In situ characterisation for studying nucleation and growth of nanostructured materials and thin films during liquid-based synthesis

Kristine Bakken, Ola Gjønnes Grendal, Mari-Ann Einarsrud

Abstract

Abstract Knowledge about the nucleation, growth, and formation mechanisms during materials synthesis using sol-gel and solution-based methods is important to design a material with desired properties. We used aqueous chemical synthesis as an environmentally friendly and highly flexible route to tailored and reproducible synthesis of oxide nanomaterials and thin films. For studies of hydrothermal synthesis an in situ cell using synchrotron X-ray diffraction was used to investigate the formation mechanisms of SrxBa1-xNb2O6 piezoelectrics. Aqueous chemical solution deposition of phase pure oriented piezoelectric thin films demands strong control of processing parameters. An in situ cell for synchrotron X-ray diffraction studies of the annealing and crystallisation steps during aqueous chemical solution deposition was used to understand the nucleation and crystallisation of Ba0.85Ca0.15Zr0.1Ti0.9O3 (BCZT). We discuss how the knowledge about nucleation and growth obtained by in situ characterisation can be used to design the optimal procedure for fabrication of oxide materials with desired properties.
Source: crossref · Quality: baseline

Research context

OpenAlex topics: Ferroelectric and Piezoelectric Materials · Acoustic Wave Resonator Technologies · Electronic and Structural Properties of Oxides

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

References (45)

Show source-provided references
1. Polak E, Munn J, Barnes P, Tarling SE, Ritter C (1990) Time-resolved neutron diffraction analyses of hydrothermal syntheses using a novel autoclave cell. J Appl Cryst. https://doi.org/10.1107/S002188989000247310.1107/S0021889890002473 ↗
2. Bremholm M, Felicissimo M, Iversen BB (2009) Time-resolved in situ synchrotron X-ray study and large-scale production of magnetite nanoparticles in supercritical water. Angew Chemie Int Ed. https://doi.org/10.1002/anie.20090104810.1002/anie.200901048 ↗
3. Tyrsted C, Becker J, Hald P, Bremholm M, Pedersen JS, Chevallier J, Cerenius Y, Iversen SB, Iversen BB (2010) In-situ synchrotron radiation study of formation and growth of crystalline CexZr1−xO2 nanoparticles synthesized in supercritical water. Chem Mater. https://doi.org/10.1021/cm903316s10.1021/cm903316s ↗
4. Tyrsted C, Jensen KMO, Bøjesen ED, Lock N, Christensen M, Billinge SJL, Iversen BB. (2012) Understanding the formation and evolution of ceria nanoparticles under hydrothermal conditions. Angew Chemie. https://doi.org/10.1002/ange.20120474710.1002/ange.201204747 ↗
5. Dippel AC, Jensen KMO, Tyrsted C, Bremholm M, Bojesen ED, Saha D, Birgisson S, Christensen M, Billinge SJL, Iversen BB. (2016) Towards atomistic understanding of polymorphism in the solvothermal synthesis of ZrO2 nanoparticles. Acta Crystallography A. https://doi.org/10.1107/S205327331601267510.1107/S2053273316012675 ↗
6. Juelsholt M, Lindahl Christiansen T, Jensen KMØ. (2019) Mechanisms for tungsten oxide nanoparticle formation in solvothermal synthesis: from polyoxometalates to crystalline materials. J Phys Chem C. https://doi.org/10.1021/acs.jpcc.8b1239510.1021/acs.jpcc.8b12395 ↗
7. Hinterberger S, Tscheließnig R, Jungbauer A. (2018) Anisotropic assembly during heat-up: the early stage hydrothermal synthesis of TiO2 from a complexed precursor. ChemNanoMat. https://doi.org/10.1002/cnma.20180032610.1002/cnma.201800326 ↗
8. Chen J, Bai J, Chen H, Graetz J. (2011) In situ hydrothermal synthesis of LiFePO4 studied by synchrotron X-ray diffraction. J Phys Chem Letters. https://doi.org/10.1021/jz200820910.1021/jz2008209 ↗
9. Birgisson S, Jensen KMO, Christiansen TL, von Bulow JF, Iversen BB. (2014) In situ powder X-ray diffraction study of the hydro-thermal formation of LiMn2O4 nanocrystallites. Dalton Trans. https://doi.org/10.1039/C4DT01307G10.1039/C4DT01307G ↗
10. Bøjesen ED, Jensen KMØ, Tyrsted C, Mamakhel A, Andersen HL, Reardon H, Chevalier J, Dippel AC, Iversen BB. (2026) The chemistry of ZnWO4 nanoparticle formation. Chem Sci. https://doi.org/10.1039/C6SC01580H10.1039/C6SC01580H ↗
11. Walton RI, Millange F, Smith RI, Hansen TC, O’Hare D. (2001) Real time observation of the hydrothermal crystallisation of barium titanate using in situ neutron powder diffraction. J Am Chem Soc. https://doi.org/10.1021/ja011805p10.1021/ja011805p ↗
12. Skjærvø SL, Sommer S, Nørby P, Bøjesen ED, Grande T, Iversen BB, Einarsrud MA. (2017) Formation mechanism and growth of MNbO3, M=K, Na by in situ X-ray diffraction. J Am Chem Soc. https://doi.org/10.1111/jace.1493210.1111/jace.14932 ↗
13. Skjærvø SL, Wells KH, van Beek W, Grande T, Einarsrud MA. (2018) Kinetics during hydrothermal synthesis of nanosized KxNa1−xNbO3. CrystEngComm. https://doi.org/10.1039/C8CE01178H10.1039/C8CE01178H ↗
14. Hertl W. (1988) Kinetics of barium titanate synthesis. J Am Chem Soc. https://doi.org/10.1111/j.1151-2916.1988.tb07540.x10.1111/j.1151-2916.1988.tb07540.x ↗
15. Dalod ARM, Grendal OG, Skjærvø SL, Inzani K, Selbach SM, Henriksen L, van Beek W, Grande T, Einarsrud MA. (2017) Controlling oriented attachment and in situ functionalisation of TiO2 nanoparticles during hydrothermal synthesis with APTES. J Phys Chem C. https://doi.org/10.1021/acs.jpcc.7b0260410.1021/acs.jpcc.7b02604 ↗
16. Grendal OG, Nylund IE, Blichfeld AB, Tominaka S, Ohara K, Selbach SM, Grande T, Einarsrud MA (2020) Controlled growth of SrxBa1-xNb2O6 hopper- and cube-shaped nanostructures by hydrothermal synthesis. Chem. Eur. J. https://doi.org/10.1002/chem.20200037310.1002/chem.202000373 ↗
17. Schwartz RW, Schneller T, Waser R. (2004) Chemical solution deposition of electronic oxide films. Comptes Rendus Chimie. https://doi.org/10.1016/j.crci.2004.01.00710.1016/j.crci.2004.01.007 ↗
18. Bassiri-Gharb N, Bastani Y, Bernal A (2014) Chemical solution growth of ferroelectric oxide thin films and nanostructures. Chem Soc Rev. https://doi.org/10.1039/C3CS60250H10.1039/C3CS60250H ↗
19. Acosta M, Novak N, Rojas V, Patel S, Vaish R, Koruza J, Rossetti GA, Rödel J (2017) BaTiO3-based piezoelectrics: Fundamentals, current status, and perspectives. Appl Phys Rev. https://doi.org/10.1063/1.499004610.1063/1.4990046 ↗
20. Bauer S, Rodrigues A, Baumbach T (2018) Real time in situ X-ray diffraction study of the crystalline structure modification of Ba0.5Sr0.5TiO3 during post-annealing. Sci Rep. https://doi.org/10.1038/s41598-018-30392-y10.1038/s41598-018-30392-y ↗
21. Roelsgaard M, Dippel AC, Andersen Borup K, Nielsen IG, Nyborg Broge N, Röh JT, Gutowski O, Iversen BB (2019) Time-resolved grazing-incidence pair distribution functional during deposition by radio-frequency magnetron sputtering. IUCrJ. https://doi.org/10.1107/S205225251900119210.1107/S2052252519001192 ↗
22. Kaune G, Hartnauer S, Scheer R (2014) In situ XRD investigation of Cu2ZnSnSe4 thin film growth by co-evaporation. Phys Status Solidi. https://doi.org/10.1002/pssa.20133034010.1002/pssa.201330340 ↗
23. Bertram F, Deiter C, Pflaum K, Suendorf M, Otte C, Wollsshläger J (2011) In-situ X-ray diffraction studies on post-deposition vacuum-annealing of ultra-thin iron oxide films. J Appl Phys. https://doi.org/10.1063/1.366165510.1063/1.3661655 ↗
24. Davydok A, Cornelius TW, Mocuta C, Lima EC, Araujo EB, Thomas O (2016) In situ X-ray diffraction studies on the piezoelectric response of PZT thin films. Thin Solid Films. https://doi.org/10.1016/j.tsf.2016.01.04510.1016/j.tsf.2016.01.045 ↗
25. Jensen KMØ, Blichfeld BB, Bauers SR, Wood SR, Doooryhee E, Johnson DC, Iversen BB, Billinge SJ (2015) Demonstration of thin film pair distribution function analysis (tfPDF) for the study of local structure in amorphous and crystalline thin films. IUCrJ. https://doi.org/10.1107/S205225251501222110.1107/S2052252515012221 ↗
26. Dippel AC, Roelsgaard M, Boettger U, Schneller T, Gutowski O, Ruett U (2019) Local atomic tructure of thin and ultrathinfils via rapid high-energy X-ray total scattering at grazing incidence. IUCrJ. https://doi.org/10.1107/S205225251900051410.1107/S2052252519000514 ↗
27. Nittala K, Mhin S, Jones JL, Robinson DS, Ihlefeld JF, Brennecka GL (2012) In situ X-ray diffraction of solution-derived ferroelectric thin films for queantitiative phase and texture evolution mearurement. J Appl Phys. https://doi.org/10.1063/1.476638710.1063/1.4766387 ↗
28. Nittala K, Mhin S, Dunnigan KM, Robinson DS, Ihlefeld JF, Kotula PG, Brennecka GL, Jones JL (2013) Phase and texture evolution in solution deposited lead zirconate titanate thin films: Formation and role of the Pt3Pb intermetallic phase. J Appl Phys. https://doi.org/10.1063/1.481168710.1063/1.4811687 ↗
29. Blichfeld AB, Bakken K, Chernyshov D, Glaum J, Grande T, Einarsrud MA (2020) Experimental setup for high-temperature in situ studies of crystallisation of thin films with atmospheric control. J Synchrotron Rad. https://doi.org/10.1107/S160057752001014010.1107/S1600577520010140 ↗
30. Bakken K, Blichfeld AB, Chernyshov D, Grande T, Glaum J, Einarsrud MA (2020) Mechanisms for texture in BaTiO3 thin films from aqueous chemical solution deposition. J Sol-Gel Sci Tech. https://doi.org/10.1007/s10971-020-05356-210.1007/s10971-020-05356-2 ↗
31. Bakken K, Pedersen VH, Blichfeld AB, Nylund IE, Tominaka S, Ohara K, Grande T, Einarsrud MA (2021) Structures and role of the intermediate phased on the crystallisation of BaTiO3 from an aqueous synthesis route. ACS Omega. https://doi.org/10.1021/acsomega.1c0008910.1021/acsomega.1c00089 ↗
32. Bakken K, Blichfeld AB, Nylund IE, Chernyshov D, Glaum J, Grande T, Einarsrud MA (2021) Tailoring preferential orientation in BaTiO3-based thin films from aqueous chemical solution deposition. Chemistry-Methods. https://doi.org/10.1002/cmtd.20210006410.1002/cmtd.202100064 ↗
33. Bakken K, Gaukås NH, Grendal OG, Blichfeld AB, Tominaka S, Ohara K, Chernyshov D, Glaum J, Grande T, Einarsrud MA (2021) In situ X-ray diffraction studies of the crystallisation of K0.5Na0.5NbO3 powders and thin films from an aqueous synthesis route. Open Ceramics. https://doi.org/10.1016/j.oceram.2021.10014710.1016/j.oceram.2021.100147 ↗
34. Pedersen VH, Blichfeld AB, Bakken K, Chernyshov D, Grande T, Einarsrud MA (2022) Crystallisation and texturing of Sr1-xBaxNb2O6 thin films prepared by aqueous solution deposition – An in situ X-ray diffraction study. Cryst Growth Des. https://doi.org/10.1021/acs.cgd.2c0055310.1021/acs.cgd.2c00553 ↗
35. Grendal OG, Blichfeld AB, Vu TD, van Beek W, Selbach SM, Grande T, Einarsrud MA (2019) Composition and morphology tuning during hydrothermal synthesis of SrxBa1-xNb2O6 tetragonal tungsten bronzes studied by in situ X-ray diffraction. CrystEngComm. https://doi.org/10.1039/C9CE01049A10.1039/C9CE01049A ↗
36. Becker J, Bremholm M, Tyrsted C, Pauw B, Jensen KMØ, Eltzholt J, Christensen M, Iversen BB (2010) Experimental setup for in situ X-ray SAXA/WAXS/PDF studies of the formation and growth of nanoparticles in near- and supercritical fluids. J. Appl. Crystallogr. https://doi.org/10.1107/S002188981001468810.1107/S0021889810014688 ↗
37. Dyadkin V, Pattison P, Dmitriev V, Chernyshov D (2016) A new multipurpose diffractometer PILATUS@SNBL. J Synchrotron Radiat. https://doi.org/10.1107/S160057751600241110.1107/S1600577516002411 ↗
38. Khomyakova E, Wenner S, Bakken K, Schultheiss J, Grande T, Glaum J, Einarsrud MA (2020) On the formation mechanism of Ba0.85Ca0.15Zr0.1Ti0.9O3 thin films by aqueous chemical solution deposition. J Eur Cer Soc. https://doi.org/10.1016/j.jeurceramsoc.2020.07.04210.1016/j.jeurceramsoc.2020.07.042 ↗
39. Lutterotti L (2010) Total pattern fitting for the combined size-strain-stress-texture determination in thin film diffraction. Nucl Inst Meth Phys Res Section B: Beam Inter Mat Atoms. https://doi.org/10.1016/j.nimb.2009.09.05310.1016/j.nimb.2009.09.053 ↗
40. Hielscher R, Schaaben H (2008) A novel pole figure inversion method: Specification of the MTEX algorithm. J Appl Cryst. https://doi.org/10.1107/S002188980803011210.1107/S0021889808030112 ↗
41. Bera J, Rout SK (2005) On the formation mechanism of BaTiO3-BaZrO3 solid solution through solid-oxide reaction. Mat Lett. https://doi.org/10.1016/j.matlet.2004.07.05310.1016/j.matlet.2004.07.053 ↗
42. El-Kaderi HM, Hunt JR, Mendoza-Cortés JL, Côté AP, Taylor RE, Keeffe M, Yaghi OM (2007) Designed synthesis of 3D covalent organic frameworks. Science. https://doi.org/10.1126/science.113991510.1126/science.1139915 ↗
43. Bøjesen ED, Iversen BB (2016) The chemistry of nucleation. CrystEngComm. https://doi.org/10.1039/C6CE01489E10.1039/C6CE01489E ↗
44. Gaukås NH, Dale SM, Ræder TM, Toresen A, Holmestad R, Glaum J, Einarsrud MA, Grande T (2019) Controlling phase purity and texture of K0.5Na0.5NbO3 thin films by aqueous chemical solution deposition. Materials. https://doi.org/10.3390/ma1213204210.3390/ma12132042 ↗
45. Christensen M, Einarsrud MA, Grande T (2017) Fabrication of lead-free Bi0.5Na0.5TiO3 thin films by aqueous chemical solution deposition. Materials. https://doi.org/10.3390/ma1002021310.3390/ma10020213 ↗