In-situ GISAXS investigation of the structure evolution mechanism of template removal of ordered mesoporous films prepared via a soft-templating method
Source abstract
Abstract
Abstract The soft-templating method is important in the preparation of ordered mesoporous carbon materials. In the process, careful removal of the block template is a critical step in obtaining a highly ordered mesostructure before carbonization. In this study, the dynamic structure evolution of template removal by means of calcination using both high (3 °C/min) and low (1 °C/min) heating rates was monitored using an in situ GISAXS technique. The real-time d-spacing and order degree parameters including the mesochannel dislocation and grain size of the ordered structure were determined as a function of calcination time. The results showed that the entire structure evolution process could be divided into three stages according to variable rates of d-spacing: glass transition stage, molten phase transition stage, and pyrolysis stage. In the first stage, thermal expansion transition into template shrinkage was observed as the polymer chain transitioned from a rigid to a softer state. Shrinkage of the template occurred, while a highly ordered mesostructured remained. In the second stage, the template became flexible after the molten phase transition, and the rate of structure change gradually increased, accompanied by mesochannel dislocation. Fast pyrolysis occurred in the last stage, the ordered structure was destroyed, and internal stress was released. This phenomenon was also clearly observed when the heating rate was 3 °C/min. The final ratio of dislocation comparing the state before and after template removal was 9.13, which is significantly higher than the value of 5.84 observed with a heating rate of 1 °C/min. The results indicated that the ordered mesostructure after template removal was determined by not only the critical temperature but also the heating profile during the entire process of structure evolution. A hypothetical mechanism is proposed to explain the structure evolution of template removal for ordered mesoporous films prepared by a soft-templating method. A reasonable design for a heating profile for template removal based on this in situ GISAXS study can be an effective method for improving the quality of mesoporous films.
Source: openaire · Quality: candidate unverified · Source record ↗
Research context
OpenAlex topics: Mesoporous Materials and Catalysis · Advanced ceramic materials synthesis · Supercapacitor Materials and Fabrication
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (55)
Show source-provided references
1. Scalable synthesis of honeycomb-like ordered mesoporous carbon nanosheets and their application in lithium–sulfur batteries10.1021/acsami.6b13370 ↗
2. Mesoporous MoS2 as a transition metal dichalcogenide exhibiting pseudocapacitive Li and Na-ion charge storage10.1002/aenm.201501937 ↗
3. Hierarchically ordered mesoporous Co 3 O 4 materials for high performance Li-ion batteries
4. Graphene-based ordered mesoporous carbon hybrids with large surface areas for supercapacitors10.1039/C7NJ03923A ↗
5. Synthesis and supercapacitor performance of polyaniline/nitrogen-doped ordered mesoporous carbon composites10.1186/s11671-018-2577-3 ↗
6. Two-dimensional gold trisoctahedron nanoparticle superlattice sheets: self-assembly, characterization and immunosensing applications10.1039/C7NR09443D ↗
7. Ordered mesoporous carbon and its applications for electrochemical energy storage and conversion10.1039/C6QM00298F ↗
8. Mesoporous carbon nanomaterials in drug delivery and biomedical application10.1080/10717544.2017.1399300 ↗
9. Mesoporous silica nanoparticles for drug delivery and biosensing applications10.1002/adfm.200601191 ↗
10. Sensing heavy metals using mesoporous-based optical chemical sensors
11. PtNi nanoalloys-loaded ordered mesoporous carbon for high-capacity hydrogen storage10.1080/10667857.2017.1278899 ↗
12. Surfactant-assisted nanocasting route for synthesis of highly ordered mesoporous graphitic carbon and its application in CO 2 adsorption
13. A general soft-enveloping strategy in the templating synthesis of mesoporous metal nanostructures10.1038/s41467-018-02930-9 ↗
14. Constrained growth of MoS2 nanosheets within a mesoporous silica shell and its effects on defect sites and catalyst stability for H2S decomposition10.1021/acscatal.7b03123 ↗
15. Three-dimensional ordered mesoporous Co 3 O 4 enhanced by Pd for oxygen evolution reaction
16. Direct synthesis of ordered mesoporous hydrothermal carbon materials via a modified soft-templating method10.1016/j.micromeso.2017.07.001 ↗
17. Fabrication of continuous mesoporous carbon films with face-centered orthorhombic symmetry through a soft templating pathway10.1039/b705692c ↗
18. Recent progress in soft-templating of porous carbon materials10.1039/c2sm07448f ↗
19. Synthesis of a large-scale highly ordered porous carbon film by self-assembly of block copolymers10.1002/anie.200461051 ↗
20. Synthesis of mesoporous carbon materials via enhanced hydrogen-bonding interaction10.1021/ja060242k ↗
21. A facile aqueous route to synthesize highly ordered mesoporous polymers and carbon frameworks with Ia3̄d bicontinuous cubic structure10.1021/ja0545721 ↗
22. Ordered mesoporous silicas and carbons with large accessible pores templated from amphiphilic diblock copolymer poly(ethylene oxide)-b-polystyrene10.1021/ja067379v ↗
23. Salt-induced phase separation to synthesize ordered mesoporous carbon by pH-controlled self-assembly10.1021/acs.jpcc.6b11056 ↗
24. Morphology evolution in mesoporous titania block copolymer composite films with increasing sol–gel reaction time10.1002/ejic.201201366 ↗
25. Structure evolution of ordered mesoporous carbons induced by water content of mixed solvents water/ethanol10.1186/s11671-016-1569-4 ↗
26. Effect of post-treatment on ordered mesoporous silica antireflective coating10.1039/C4RA06788F ↗
27. Investigation of the effect of calcination temperature on HMDS-treated ordered mesoporous silica film10.1016/j.jcis.2008.07.024 ↗
28. In situ SAXS study on a new mechanism for mesostructure formation of ordered mesoporous carbons: thermally induced self-assembly10.1021/ja208941s ↗
29. Relationship between crosslinking and ordering kinetics for the fabrication of soft templated (FDU-16) mesoporous carbon thin films10.1039/C4RA08316D ↗
30. A family of highly ordered mesoporous polymer resin and carbon structures from organic− organic self-assembly10.1021/cm060921u ↗
31. Using three-dimensional 3D grazing-incidence small-angle x-ray scattering (GISAXS) analysis to probe pore deformation in mesoporous silica films10.1021/am404602t ↗
32. Challenges in fabrication of mesoporous carbon films with ordered cylindrical pores via phenolic oligomer self-assembly with triblock copolymers10.1021/nn9012884 ↗
33. Operando grazing incidence small-angle X-ray scattering/X-ray diffraction of model ordered mesoporous Lithium-ion battery anodes10.1021/acsnano.6b06708 ↗
34. In-situ GISAXS investigation of pore orientation effects on the thermal transformation mechanism in mesoporous titania thin films10.1021/jp406165v ↗
35. Probing surface and interface morphology with grazing incidence small angle X-ray scattering10.1016/j.surfrep.2009.07.002 ↗
36. Atomic layer deposition-based tuning of the pore size in mesoporous thin films studied by in situ grazing incidence small angle X-ray scattering10.1039/C4NR05049E ↗
37. In situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films10.1021/acs.jpcc.5b06945 ↗
38. A new device for high-temperature in situ GISAXS measurements10.1063/1.5005879 ↗
39. X-ray standing wave enhanced scattering from mesoporous silica thin films10.1063/1.4974922 ↗
40. Self-assembly and crystallization behavior of mesoporous, crystalline HfO2 thin films: a model system for the generation of mesostructured transition-metal oxides10.1002/smll.200500024 ↗
41. Pyrolysis, crystallization, and sintering of mesostructured Titania thin films assessed by in situ thermal ellipsometry10.1021/ja078140x ↗
42. Ordered mesoporous polymers and homologous carbon frameworks: amphiphilic surfactant templating and direct transformation10.1002/ange.200501561 ↗
43. A facile method to prepare macroscopically oriented mesostructured silica film: controlling the orientation of mesochannels in multilayer films by air flow10.1021/ja8003254 ↗
44. A general model for estimating the ordering of mesoporous film by grazing incidence small angle X-ray scattering10.1063/1.4875662 ↗
45. Scattering curves of ordered mesoscopic materials10.1021/jp0467494 ↗
46. Diffraction line-shape analysis of poly (3-dodecylthiophene): a study of layer disorder through the liquid crystalline polymer transition10.1021/ma981059h ↗
47. Quantitative analysis of lattice disorder and crystallite size in organic semiconductor thin films10.1103/PhysRevB.84.045203 ↗
48. A general relationship between disorder, aggregation and charge transport in conjugated polymers10.1038/nmat3722 ↗
49. Grazing-incidence transmission X-ray scattering: surface scattering in the born approximation10.1107/S0021889812047887 ↗
50. Pore shape and sorption behaviour in mesoporous ordered silica films10.1107/S1600576716013698 ↗
51. Two-dimensional-hexagonal periodic mesoporous polymer resin thin films by soft templating10.1021/cm901163t ↗
52. Unidirectional self-assembly of soft templated mesoporous carbons by zone annealing10.1039/c3nr02821f ↗
53. Control of ordering and structure in soft templated mesoporous carbon films by use of selective solvent additives10.1021/la401505h ↗
54. Molecular weight dependence of reductions in the glass transition temperature of thin, freely standing polymer films10.1103/PhysRevE.63.031801 ↗
55. Confinement effects on glass transition temperature, transition breadth, and linear expansivity: an ultraslow X-ray reflectivity study on supported ultrathin polystyrene films10.1140/epje/i2013-13066-3 ↗