Salt melt synthesis of ceramics, semiconductors and carbon nanostructures

Liu, Xiaofeng; Fechler, Nina; Antonietti, Markus

doi:10.1039/c3cs60159e

Cited by 575 publications

(473 citation statements)

References 195 publications

(173 reference statements)

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“…Convective liquid fluxes (salts, metals, or oxides) can serve as reaction media that aid diffusion and enable rapid formation of compounds at temperatures far below their melting points (1)(2)(3)(4)(5)(6). The flux can be nonreactive or reactive; in the latter case the flux itself becomes incorporated into the product (7,8).…”

mentioning

confidence: 99%

In situ studies of a platform for metastable inorganic crystal growth and materials discovery

Shoemaker

Chung

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

133

152

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Rapid shifts in the energy, technological, and environmental demands of materials science call for focused and efficient expansion of the library of functional inorganic compounds. To achieve the requisite efficiency, we need a materials discovery and optimization paradigm that can rapidly reveal all possible compounds for a given reaction and composition space. Here we provide such a paradigm via in situ X-ray diffraction measurements spanning solid, liquid flux, and recrystallization processes. We identify four new ternary sulfides from reactive salt fluxes in a matter of hours, simultaneously revealing routes for ex situ synthesis and crystal growth. Changing the flux chemistry, here accomplished by increasing sulfur content, permits comparison of the allowable crystalline building blocks in each reaction space. The speed and structural information inherent to this method of in situ synthesis provide an experimental complement to computational efforts to predict new compounds and uncover routes to targeted materials by design.D iscovering new materials is a crucial step to address largescale problems of energy conversion, storage, and transmission and other technological needs whether seeking bulk phases or thin films. Dense inorganic materials are desired for their tunable transport, magnetism, optical absorption, and stability, but their existence in general cannot be predicted with the near certainty of that of metastable organic and organometallic compounds. Whereas the desire to efficiently locate and assemble inorganic materials is great, it is hindered by traditional solid-state synthetic methods-at high temperatures often only the energy-minimum thermodynamic product is obtained. To strive toward an arena where metastable compounds can be discovered rapidly and made systematically, here we conduct reactions within liquid fluxes and use in situ monitoring to capture signatures of new phases, even when they quickly dissolve in the melt.Convective liquid fluxes (salts, metals, or oxides) can serve as reaction media that aid diffusion and enable rapid formation of compounds at temperatures far below their melting points (1-6). The flux can be nonreactive or reactive; in the latter case the flux itself becomes incorporated into the product (7,8). This wellestablished approach has demonstrated the prolific discovery of novel inorganic materials grown out of low-melting fluxes, from oxides and other chalcogenides (9-12), to pnictides (13,14), to intermetallics (15), many of which cannot be attained by direct combinations of the elements. Despite the variety of metastable phases formed in these reactions, the classical approach is to predetermine a given set of reaction conditions (e.g., time, temperature, and heating and cooling rates) and wait for completion to isolate and identify the formed compounds. It is not possible to observe how the reaction system itself has arrived at the isolated compound, whether the crystalline material formed on heating, on cooling, or on soaking at the given high temperature,...

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mentioning

confidence: 99%

In situ studies of a platform for metastable inorganic crystal growth and materials discovery

Shoemaker

Chung

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

133

152

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“…For more information regarding the preparation of porous carbon materials via ionothermal/ molten salt approaches and also their main applications, several review works are available in the literature [132][133][134][135][136].…”

Section: Porosity -Process Technologies and Applicationsmentioning

confidence: 99%

Nanoporous Carbon Synthesis: An Old Story with Exciting New Chapters

Mestre¹,

Carvalho²

2018

Porosity - Process, Technologies and Applications

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Activated carbons are key materials in technological applications of multidisciplinary fields (e.g. adsorption, separation, and catalytic processes). The extensive use of these materials results from the combination of a well-developed pore network (micropores or micro + mesopores) along with the presence of heteroatoms (e.g. oxygen, nitrogen, and sulfur). The large scale production of nanoporous carbons is a well-established process since the first patents date from the beginning of the twentieth century. Conventional activation methodologies are divided between physical, using steam or CO 2 , and chemical, being KOH, ZnCl 2 , and H 3 PO 4 the most commonly reported oxidizing agents. Due to the panoply of operational parameters that can be changed or added in the production of activated carbons, there is still room for R&D. In this chapter, both conventional and innovative synthetic processes are reviewed to offer an up-to-date picture regarding raw materials, carbonization step, activation process, and other approaches. Conventional activation of gels and chars obtained by novel approaches (i.e. sol-gel method, hydrothermal carbonization (HTC), and acid-mediated carbonization) and more innovative strategies (i.e. variations of HTC process, carbonization of organic salts and ionothermal approaches) are addressed. Textural, surface chemistry and morphological properties of the derived porous carbons were reviewed and critically rationalized.

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“…Furthermore, MSS is good at solvating metals and oxides at high temperature owing to a destabilization of bonding by the strong polarizing forces provided by the salt melts. MSS has the additional advantage of low cost and low toxicity as well as abundant availability 10 .…”

Section: Fast and Scalable Synthesis Of Strontium Niobates With Contrmentioning

confidence: 99%

Fast and scalable synthesis of strontium niobates with controlled stoichiometry

2017

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Link to publication record in Explore Bristol Research PDF-document This is the author accepted manuscript (AAM). The final published version (version of record) is available online via RSC at http://pubs.rsc.org/en/Content/ArticleLanding/2017/CE/C7CE01298E#!divAbstract. Please refer to any applicable terms of use of the publisher. University of Bristol -Explore Bristol Research General rightsThis document is made available in accordance with publisher policies. Please cite only the published version using the reference above. Full terms of use are available:

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Salt melt synthesis of ceramics, semiconductors and carbon nanostructures

Cited by 575 publications

References 195 publications

In situ studies of a platform for metastable inorganic crystal growth and materials discovery

In situ studies of a platform for metastable inorganic crystal growth and materials discovery

Nanoporous Carbon Synthesis: An Old Story with Exciting New Chapters

Fast and scalable synthesis of strontium niobates with controlled stoichiometry

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