Nanomaterial composition and method for producing same

Abstract

A nanoparticle composition, an electrospun nonwoven material composition, and a method for making the same are disclosed. The nanoparticles can be made by electrospinning a composition comprising a sacrificial polymer and a first and a second ionic species into a fiber and decomposing at least a portion of the sacrificial polymer. The nanoparticles can include an electroactive compound. The nanoparticles can include a catalytically active compound. The nanoparticles can further be included in the composition prepared as a nonwoven material. The nonwoven material can be used to prepare a battery composition. The battery composition can include an electrode comprising the nanoparticles.

Description

[Technical field]

[0001] [CROSS-REFERENCE TO RELATED APPLICATIONS] This application claims the benefit of U.S. Provisional Application No. 63 / 285,903, filed December 03, 2021, the disclosure of which is incorporated herein by reference in its entirety.

[0002] FIELD OF THE DISCLOSURE The present disclosure relates to nanomaterial compositions and methods of making and using same. In particular, the present disclosure relates to nonwoven material compositions and methods of making and using same. The present disclosure further relates to particulate compositions and methods of making and using same. [Background technology]

[0003] Nanomaterials, such as nanoparticles, are becoming ubiquitous in consumer and industrial products. However, the nano- and / or mesostructure of nanomaterials directly impacts their performance in various applications, such as electrode assemblies and catalysis. For example, small nanoparticles tend to have higher catalytic efficiency due to their larger surface area to volume ratio compared to larger nanoparticles. Furthermore, smaller nanoparticles are less prone to dislocations and other crystal deformations, making them desirable for use in electrode assemblies. Furthermore, the mesostructure of electrode assemblies containing nanoparticles can greatly affect the electrochemical performance of the assemblies. For example, electrodes containing high aspect ratio nanomaterials show promise for use in high performance lithium-ion batteries.

[0004] The manufacturing method of nanomaterials affects the nanostructure, mesostructure, and morphology distribution of nanomaterials. Nanoparticles can be manufactured by top-down methods, which reduce macrostructures to nanostructures, or by bottom-up methods, which build nanostructures from atoms. Top-down methods produce relatively large nanoparticles with non-uniform distribution of size and morphology, while generating a lot of waste. Common bottom-up methods include flame reactor processes, plasma reactor processes, laser reactor processes, hot wall reactor processes, chemical or vapor deposition methods, precipitation methods, and sol-gel processes. These manufacturing methods often require harsh conditions, produce nanoparticles with non-uniform distribution of size and morphology, require optimization of reaction kinetics, or require extensive post-processing to isolate the nanoparticles. For nanomaterial-containing electrodes, traditional preparation has been performed by slurry casting. However, slurry casting leads to the formation of non-uniform mesostructures, which results in slow electron transport.

[0005] Further improvements in the processes for producing nanoparticles are needed. Additionally, there is a need for improved electroactive nanomaterials and processes for producing such nanomaterials. Summary of the Invention [Problem to be solved by the invention]

[0006] In one aspect, the present disclosure describes a composition comprising an electrospun nonwoven material. The nonwoven material comprises fibers having an average diameter of less than 5 μm. The fibers comprise a sacrificial polymer present at 40% to 60% by weight of the total weight of the electrospun nonwoven material, and a first ionic species and a second ionic species dispersed on the sacrificial polymer and distributed along the fibers, the first ionic species and the second ionic species being ionic species of at least one salt, the at least one salt being present at 60% or less by weight of total salt, and the weight % of the total salt relative to the weight % of the sacrificial polymer is greater than or equal to 1 part by weight of the total salt relative to 6 parts by weight of the sacrificial polymer.

[0007] The at least one salt may include NiCl2, Ni(CH3COO)2, ZnSO4, Zn(CH3COO)2, KCl, KAuCl4, CoCl2, Co(CH3COO)2, CuCl2, Cu(NO3)2, PdCl6, K2PdCl6, Na2PtCl4, K2PtBr4, Ni(NO3)2, Co(NO3)2, Mn(NO3)2, Al(NO3)3, Fe(NO3)2, LiNO3, LiH2PO4, Fe(CH3COO)2, NiSO4, CoSO4, Li2SO4, MnSO4, FeSO4, Al2(SO4)3, Al(OCH3)3, Al(CH3COO)3, or combinations thereof.

[0008] The sacrificial polymer may be polyvinylpyrrolidone, polyethylene glycol, nylon, polyurethane, polyvinyl alcohol, polyvinyl acetate, polyacrylonitrile, polyacrylate, or combinations thereof.

[0009] The weight percent of the total salt to the weight percent of the sacrificial polymer may be from 1:6 to 2:1, from 1:3 to 5:3, from 2:3 to 5:3, from 2:3 to 4:3, or from 1:3 to 4:3.

[0010] The composition comprising an electrospun nonwoven layer comprises a substrate and fibers deposited on the substrate by electrospinning. The fibers comprise a polymer and a plurality of nanoparticles dispersed on the polymer and distributed throughout the fibers, the plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm, and each nanoparticle comprises a plurality of at least one chemical species. A plurality of fibers may form the first fiber layer. The composition may further comprise a second fiber layer comprising a second fiber deposited on the first fiber layer by electrospinning. The second fibers comprise a second polymer and a second plurality of nanoparticles dispersed on the second polymer and distributed throughout the fibers, the second plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm, and each nanoparticle comprises a plurality of at least one chemical species, and the first fiber layer has a density at least 1.1 times the density of the second fiber layer.

[0011] The plurality of nanoparticles may be a first plurality of nanoparticles, each nanoparticle comprising a first chemical species, and the composition may further comprise a second plurality of nanoparticles, each nanoparticle comprising a second chemical species different from the first chemical species.

[0012] The fibers may have an average diameter of less than 1 μm. The polymer may be a binder polymer. The polymer may include one or more polyamides, polysulfones, polyethers, polyesters, polyamines, polyalcohols, polyurethanes, polycarbonates, polyaromatics, photopolymers, polyimides, polyacrylates, polyvinylidene fluorides, or combinations thereof.

[0013] The electrospun nonwoven layer may further include a conductive material. The conductive material may be carbon powder. The substrate may be a current collector. The substrate may include Cu foil, Al foil, Pt foil, Ni foil, a woven substrate, a nonwoven substrate, an artificial solid electrolyte interface, or a combination thereof.

[0014] At least one chemical species may be electroactive. The at least one chemical species may be LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, Li(Ni x Al y Co z )O2, or combinations thereof, where x+y+z=1. At least one chemical species may be catalytically active. The at least one chemical species may include PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, TiO2, NiO, or combinations thereof.

[0015] The battery may include an electrode comprising any of the compositions described above.

[0016] The battery may include an electrode comprising a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one electroactive compound species, the plurality of nanoparticles having a particle size in the range of 0.01 μm to 0.5 μm. The electrode may include a substrate and an electrospun nonwoven layer comprising fibers deposited on the substrate by electrospinning, the fibers comprising a binder polymer and the plurality of nanoparticles dispersed on the binder polymer and distributed throughout the fibers. The plurality of nanoparticles may have a particle size in the range of 0.02 μm to 0.4 μm.

[0017] The binder polymer may include one or more polyamides, polysulfones, polyethers, polyesters, polyamines, polyalcohols, polyurethanes, polycarbonates, polyaromatics, photopolymers, polyimides, or combinations thereof.

[0018] The method includes electrospinning a solution onto a substrate, the solution comprising a binder polymer, a solvent, and a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one chemical species, the plurality of nanoparticles having a particle size in the range of 0.01 μm to 0.5 μm, and producing a nonwoven layer of fibers comprising a binder polymer and the plurality of nanoparticles dispersed within the binder polymer and distributed throughout the fibers. The fibers may have an average diameter of less than 5 μm. The at least one chemical species may be electroactive. The at least one chemical species may be selected from the group consisting of LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, and Li(Ni x Al y Co z)O2, where x+y+z=1. At least one chemical species may be catalytically active. The at least one chemical species may include PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, TiO2, NiO, or combinations thereof.

[0019] The method includes dissolving at least one salt and a sacrificial polymer in a solvent to form a solution, the solution comprising the sacrificial polymer, a first ionic species, a second ionic species, and the solvent; electrospinning the solution to form a sacrificial nonwoven material comprising fibers, the fibers comprising the sacrificial polymer and the first ionic species and the second ionic species dispersed on the polymer and distributed along the fibers; and decomposing at least a portion of the sacrificial nonwoven material, resulting in a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one chemical species, the at least one chemical species comprising a reaction product of at least the first ionic species and the second ionic species, the plurality of nanoparticles having a particle size range of 0.02 μm to 0.5 μm.

[0020] The method further includes spinning a mixture comprising a binder polymer and the plurality of nanoparticles onto a substrate, wherein electrospinning of the mixture results in a second nonwoven layer comprising second fibers comprising the binder polymer and nanoparticles from the plurality of nanoparticles dispersed within the binder polymer and distributed throughout the fibers.

[0021] The at least one salt may include LiNO3, LiH2PO4, Co(NO3)2, Ni(NO3)2, Fe(NO3)2, Mn(NO3)2, Al(NO3)3, Li2SO4, CoSO4, NiSO4, FeSO4, MnSO4, Al2(SO4)3, Fe(CH3COO)2, Al(OCH3)3, Al(CH3COO)3, or combinations thereof. At least one salt may be selected from the group consisting of (NH4)AuCl4, NaAuBr, HAuCl4, KCl, KAuCl4, Na2PdCl4, K2PdBr4, PdCl6, K2PdCl6, (NH4)2PDCl4, K2PdCl4, Na2PtCl4, K2PtBr4, PtCl6, K2PtCl4, (NH4)2PtCl4, K2Pt(NO2)4, KAg(CN)2, KCu, Ni(NO3)2, Mg(NO3)2, NiCl2, PdCl2, Ni(Ac)2, NiBr2, NiI2, NiSO4, Pb(CH3COO)2, SeCl2, Se(CH3COO)2, SeBr4, The inorganic fillers may include ZnSO4, Zn(CH3COO)2, Zn(NO3)2, ZnCl2, FeCl2, FeSO4, Fe(NO3)2, RuCl3, Ru(NO3)3, RhCl3, Rh(NO3)3, IrCl4, Ir2(SO4)3, CuCl2, Cu(NO3)2, CuSO4, Cu(CH3COO)2, SnCl4, Sn(CH3COO)2, SnSO4, Sn(NO3)4, AlCl3, Al2(SO4)3, Al(NO3)3, MgCl2, MgSO4, CoCl2, Co(CH3COO)2, CoSO4, Co(NO3)2, or combinations thereof.

[0022] The sacrificial polymer may include polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, polyvinyl acetate, polyacrylonitrile, polyacrylate, polyamide, polysulfone, polyether, polyester, polyamine, polyalcohol, polyurethane, polycarbonate, polyaromatics, photopolymers, polyimides, or combinations thereof.

[0023] The decomposition step may include a heat treatment, which may include pyrolysis at 500°C to 1100°C.

[0024] The above summary of the present disclosure is not intended to describe each disclosed embodiment or every embodiment of the present disclosure. The following description more particularly describes exemplary embodiments. In several places in this application, guidance is provided through lists of examples, which examples can be used in various combinations. In each instance, the recited list serves only as a representative group and should not be interpreted as an exclusive list. [Brief description of the drawings]

[0025] The following detailed description will refer to the following figures, in which the same reference numbers may be used to identify similar / identical components in several figures, and in which the drawings are not necessarily to scale:

[0026] [Figure 1] FIG. 1 is a schematic diagram of a process used to make nanoparticles according to an embodiment. [Diagram 2] FIG. 2 is a schematic diagram of a process used to manufacture an electrode assembly according to an embodiment. [Diagram 3] FIG. 3 is a schematic diagram of a process used to manufacture a catalyst assembly according to an embodiment. [Figure 4A] FIG. 4A is a schematic cross-sectional view of a battery according to an embodiment. [Figure 4B] FIG. 4B is a schematic cross-sectional view of an electrode used in the battery of FIG. 4A. [Diagram 5] FIG. 5 is an SEM image of electrospun fibers of Solution 3 in Example 1. [Figure 6] FIG. 6 is an SEM image of electrospun fibers of Solution 5 in Example 1. [Figure 7] FIG. 7 is an SEM image of electrospun fibers of Solution 6 in Example 1. [Figure 8] FIG. 8 is a TEM image of the LiCoO2 nanoparticles formed after pyrolysis of the nonwoven layer of FIG. [Figure 9] FIG. 9 is a high-resolution TEM image of the LiCoO2 nanoparticles formed after pyrolysis. [Figure 10]FIG. 10 is an X-ray spectrum of nanoparticles of LiCoO2 formed after pyrolysis of the nonwoven layer of FIG. 5, showing excellent crystallinity and no amorphous inclusions. [Figure 11A] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 11B] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 12] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 13A] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 13B] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 13C] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 13D] 1 is a SEM image of the fiber sample prepared in Example 2. [Figure 14A] FIG. 14A is an SEM image of the cathode assembly prepared in Example 5. [Figure 14B] FIG. 14B is a plot of the measured discharge capacity of coin cells in a half-cell configuration using the cathode assembly of Example 5. [Figure 14C] FIG. 14C is a plot of the measured coulombic efficiency of a coin cell in a half-cell configuration using the cathode assembly of Example 5.

[0027] [Definition] All scientific and technical terms used herein have the meanings commonly used in the art unless otherwise specified. The definitions provided herein are intended to facilitate understanding of certain terms used frequently herein and are not intended to limit the scope of the present disclosure.

[0028] Unless otherwise specified, the terms "polymer" and "polymeric material" include, but are not limited to, organic homopolymers, copolymers, such as block, graft, random and alternating copolymers, terpolymers, and the like, and blends and modifications thereof. Furthermore, unless otherwise specified, the term "polymer" is intended to include all possible geometric configurations of the material. These configurations include, but are not limited to, isotactic, syndiotactic, and atactic symmetries.

[0029] The term "solidity" is used herein to mean the relative amount of solid material in a fibrous material and is calculated by the following formula:

number

[0030] Articles such as "a," "an," and "the" are not intended to refer to a singular entity, but rather include general classes for which specific examples can be used for illustration.

[0031] The articles "a," "an," and "the" are used interchangeably with the term "at least one." The phrases "at least one of" and "comprises at least one of" following a list refer to any one of the items in the list, as well as any combination of two or more items in the list.

[0032] As used herein, the term "or" is generally used in its ordinary sense, including "and / or," unless the content clearly dictates otherwise. The term "and / or" refers to one or all of the listed elements or a combination of two or more of the listed elements.

[0033] The recitation of numerical ranges by endpoints includes all numbers subsumed within that range (e.g., 1 to 5 includes 1, 1.5, 2, 2.75, 3, 3.80, 4, 5, etc.; or up to 10 includes 10, 9.4, 7.6, 5, 4.3, 2.9, 1.62, 0.3, etc.). When a range of values ​​is stated as "up to" or "at least" a particular value, the value is included within the range.

[0034] As used herein, "have," "having," "include," "including," "comprise," "comprising," and the like are used in their open sense and generally mean "including, but not limited to." "Consisting essentially of," "consisting of," and the like will be understood to be encompassed by "comprising," and the like. As used herein, "consisting essentially of," with respect to compositions, products, methods, and the like, means that the components of the composition, product, method, and the like are limited to the recited components and other components that do not materially affect the basic and novel characteristics of the composition, product, method, and the like.

[0035] The terms "preferred" and "preferably" refer to embodiments that may provide certain advantages, under particular circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, and is not intended to exclude other embodiments from the scope of the present disclosure, including the claims.

[0036] Any directions referred to herein, such as "top", "bottom", "left", "right", "upper", "lower", and other directions and orientations, are described herein for clarity with reference to the figures and are not intended to limit the actual device or system or the use of the device or system. The apparatus or systems described herein can be used in multiple directions and orientations.

[0037] The term "particle size" refers to the largest dimension of each particle in a representative sample of particles. Particle size can be measured using transmission electron microscopy and / or scanning electron microscopy. The measured size of each particle corresponds to a sphere that would pass through a sieve opening of the same size if the sample of interest were sieved. When a range of particle sizes is given, 70 wt% or more, 80 wt% or more, 90 wt% or more, or 95 wt% or more of the nanoparticles have a particle size within that range.

[0038] [Detailed Description of the Invention] The present disclosure relates to nanomaterials for various applications. In particular, the present disclosure relates to nanomaterials for use in electrochemical and chemical reactions. In particular, the present disclosure relates to nonwoven material compositions and methods of making and using the same. The present disclosure further relates to nanoparticle compositions and methods of making and using the same.

[0039] According to embodiments of the present disclosure, nanoparticles can be prepared from salts by electrospinning with a sacrificial polymer. Nanoparticles made by the methods of the present disclosure may exhibit a narrow distribution of nanoparticle sizes, as measured by the average diameter of the nanoparticles. The nanoparticles may have few or no dislocations or other crystal deformations. The methods described herein are highly scalable and compatible with many salts and polymer matrices. There may be other advantages not listed here.

[0040] According to one embodiment, the sacrificial nonwoven material is synthesized by electrospinning a solution of a sacrificial polymer, at least two ionic species of at least one salt, and a solvent. The sacrificial polymer provides a fiber-forming component for forming fibers contained in the sacrificial nonwoven material. The fibers include the sacrificial polymer and at least two ionic species. The at least two ionic species are attached to the polymer. The at least two ionic species are distributed throughout the fibers. According to some embodiments, the sacrificial nonwoven material is subjected to a decomposition process. The decomposition process decomposes at least a portion of the sacrificial nonwoven material, resulting in a plurality of nanoparticles. Each nanoparticle includes a plurality of at least one compound species. The compound species is a reaction product of at least two ionic species. In some embodiments, the compound species may be a reaction product of the at least two ionic species with an additional compound or ionic species. In some embodiments, the compound species and / or nanoparticles are electroactive. In some embodiments, the compound species and / or nanoparticles are catalytically active.

[0041] According to some embodiments, the nonwoven layer is produced by spinning (e.g., electrospinning) a solution of binder polymer and nanoparticles onto a substrate. The binder polymer provides the fiber-forming components for forming the fibers. The nanoparticles adhere to the binder polymer. The nanoparticles are distributed throughout the fibers. In some embodiments, the nanoparticles are obtained by electrospinning a solution of a sacrificial polymer, at least two ions of at least one salt, and a solvent, followed by a decomposition process.

[0042] According to embodiments of the present disclosure, nanoparticles may be incorporated into the non-woven layer nanomaterial. In some embodiments, the nanoparticle-containing nanomaterial may be used in an electrode assembly, such as a battery. The electrode assembly made by the methods described herein may provide a large electrode / electrolyte interfacial area to enhance electrochemical oxidation / reduction reaction kinetics. The electrode assembly may provide a controllable interfiber void volume that allows sufficient electrolyte penetration into the electrode. The electrode assembly may provide high nanoparticle content and short lithium ion transport pathways. There may also be other advantages not listed here.

[0043] According to one embodiment, the nonwoven layer comprises a plurality of nanoparticles. Each nanoparticle comprises a plurality of at least one electroactive compound species. In some embodiments, the nonwoven layer is spun (e.g., electrospun) onto a substrate that is a current collector, thereby forming an electrode assembly. In some embodiments, the electrode assembly is a cathode assembly. In some embodiments, the electrode assembly is an anode assembly. In some embodiments, the cathode assembly can be used in a battery, such as a lithium ion battery. In some embodiments, the anode assembly can be used in a battery, such as a lithium ion battery. In some embodiments, the cathode assembly and the anode assembly can be used in a battery, such as a lithium ion battery.

[0044] According to an embodiment of the present disclosure, the nanoparticles may include at least one catalytically active compound species. In some embodiments, the catalytic assemblies are manufactured by electrospinning the nanoparticles and the binder polymer to create a nonwoven layer. In some embodiments, the nonwoven layer is deposited on a substrate. In some embodiments, the catalytic assemblies do not include a substrate.

[0045] According to embodiments of the present disclosure, nanoparticles can be incorporated into nonwoven materials. In some embodiments, nanoparticle-containing materials can be used in catalytic assemblies. The electrocatalytic assemblies made by the methods described herein can provide a nonwoven layer that allows dispersion of nanoparticles with minimal agglomeration, thus increasing the surface area of ​​each nanoparticle for catalytically active compounds to catalyze a reaction. Increasing the surface area of ​​the catalyst can be economical and environmentally friendly, since less catalytic compound is needed to carry out the desired reaction. The nonwoven layer also provides a support for the catalyst. There may be other advantages not listed here.

[0046] Referring now to FIG. 1, a general process for producing nanoparticles according to one embodiment of the present disclosure is shown. At least one salt 12 and a sacrificial polymer 16 are dissolved (arrow 1) to create a solution 20. In some embodiments, one salt or multiple salts, such as two salts, three salts, four salts, five salts, six salts, seven salts, eight salts, nine salts, or ten or more salts, may be dissolved in the solution 20. In the exemplary embodiment shown in FIG. 1, an optional second salt 14 is dissolved in the solution 20. The solution 20 includes a first ionic species and a second ionic species of at least one salt. For example, as depicted in FIG. 1, in some embodiments, the solution 20 includes a first ionic species 22 from the first salt 12, a second ionic species 24 from the first salt 12, a sacrificial polymer 16, and a solvent 26. In some embodiments in which one or more additional optional salts are dissolved in the solution 20, the solution 20 includes one or more additional ionic species. For example, in some embodiments as depicted in FIG. 1, the solution 20 includes a third ionic species 21 from the optional second salt 14 and a fourth ionic species 23 from the second salt 14. A sacrificial nonwoven material 30 is produced via spinning (e.g., electrospinning) the solution 20 (arrow 2). The sacrificial nonwoven material 30 includes fibers 36. The sacrificial polymer 16 provides the fiber-forming components of the fibers 36. Thus, the fibers 36 include the sacrificial polymer 16, and a first ionic species 22, and a second ionic species 24. The first ionic species 22 and the second ionic species 24 are attached to the polymer. The first ionic species 22 and the second ionic species 24 are distributed along the fibers 36. In some embodiments, if one or more optional additional salts are dissolved in the solution, the one or more additional ionic species from the optional salts are attached to the fibers 36. In some embodiments, when the optional additional salt or salts are dissolved in solution, the optional additional ionic species or species from the optional salt or salts are distributed across the fiber 36. For example, in some embodiments, a third ionic species 21 from the second salt 14 and a fourth ionic species 23 from the second salt 14 are attached to the polymer, as depicted in Figure 1. The third ionic species 21 and the fourth ionic species 23 are distributed along the fiber 36.The sacrificial nonwoven material 30 is subjected to a decomposition process 3 to obtain a blend 40. The blend 40 includes a plurality of nanoparticles 42. The blend 40 may include decomposed or partially decomposed fibers 46. Each nanoparticle of the plurality of nanoparticles 42 includes a plurality of at least one chemical species. The chemical species is a reaction product between at least a first ionic species 22 and a second ionic species 24.

[0047] The first ionic species 22 and the second ionic species 24 result from the dissolution of at least one salt in the solution 20. In some embodiments, the first ionic species 22 and the second ionic species 24 result from the dissolution of two or more different salts in the solution 20. In some embodiments, as shown in FIG. 1, the first ionic species 22 and the second ionic species 24 result from the dissolution of the first salt 12. In some embodiments, if any additional salts are dissolved in the solution 20, the additional ionic species result from the dissolution of the additional salts. For example, in FIG. 1, the third ionic species 21 and the fourth ionic species 23 result from the dissolution of the second salt 14 in the solution 20. In some embodiments, the first salt 12 is LiNO3. In some embodiments, the solution 20 contains the first ionic species 22, Li, from the dissolution of the first salt 12, LiNO3. + and a second ion species 24, NO3 - In some embodiments, the third ionic species 21 and the fourth ionic species 24 result from the dissolution of one or more additional salts, such as the second salt 14 depicted in FIG. 1. In some embodiments, the second salt 14 is Co(NO3)2. Thus, the solution 20 contains the third ionic species Co 2+ and an optional second salt 14, additional NO3 from dissolution of Co(NO3)2. - ions. Optional additional ionic species may be present in solution 20. The additional ionic species may be from any salts added to solution 20 in addition to at least one salt or ion present in solvent 26, e.g., ionic species present in water.

[0048] Each nanoparticle 42 of the plurality of nanoparticles includes a plurality of at least one chemical species. The chemical species is a reaction product between at least the first ionic species 22 and the second ionic species 24. In some embodiments, when the nanoparticles 42 include at least one chemical species having electroactivity, the at least one salt and the optional additional salt may be any combination of salts that dissolve into ionic species that can react to form an electroactive chemical species. Additional reactive species may participate in the reaction. The additional reactive species may be part of the reaction product. Examples of additional reactive species include oxygen, sulfur, phosphorus, nitrogen, and any combination thereof.

[0049] According to one embodiment, the compound species is electroactive. In some embodiments, the electroactive compound species is a cathodically active compound. In some embodiments, the electroactive compound species includes lithium. In some embodiments, the electroactive compound species includes lithium and one or more metals. Examples of cathodically active electroactive compound species include LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2 and Li(Ni x Al y Co z)O2, where x+y+z=1. In some embodiments, the cathode active electroactive compound species is LiCoO2. In some embodiments, the cathode active electroactive compound species is LiNiO2. Examples of salts that may dissolve and produce ionic species that can react to form the cathode active electroactive compound species include, but are not limited to, LiNO3, Co(NO3)2, Ni(NO3)2, Fe(NO3)2, Mn(NO3)2, Al(NO3)3, Li2SO4, CoSO4, NiSO4, FeSO4, MnSO4, Al2(SO4)3, Li(CH3COO), Co(CH3COO)2, Ni(CH3COO)2, Fe(CH3COO)2, Fe3O(CH3COO)2, Mn(CH3OO)2, AlOH(CH3COO)2 , Al3(CH3COO)3, LiH2PO4, Co3(PO4)2, Ni3(PO4)2, FePO4, Mn3(PO4)2, AlPO4, H3PO4, triethylphosphate (CH3CH2)3PO4, Ni(NO3)2, Co(NO3)2, Mn(NO3)2, Al(NO3)3, Fe(NO3)2, LiNO3, LiH2PO4, Fe(CH3COO)2, NiSO4, CoSO4, Li2SO4, MnSO4, FeSO4, Al2(SO4)3, Al(OCH3)3, Al(CH3COO)3, and hydrates thereof. In some embodiments, the first salt 12 is LiNO3 and the second salt 14 is Co(NO3)2·6H2O. In some embodiments, the first salt 12 is LiNO3 and the second salt 14 is Ni(NO3)2·6H2O. In some embodiments, each nanoparticle in the plurality of nanoparticles 42 may include two or more electroactive compound species that are cathodically active compounds. For example, in some embodiments, the nanoparticles may include LiCoO2 and LiNiO2.

[0050] In some embodiments, the electroactive compound species is an anode active compound species. Examples of anode electroactive compound species include Co3O4, Cu2O, Li4Ti5O 12(lithium titanate), SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO, carbides thereof, and any combination thereof. Examples of metallic anode materials include Li metal, alkaline earth metals such as Mg and Ca, and Si-based compounds. The Si-based compounds may be in the form of Si fibers. Further examples of anode electroactive species include LiAl alloys, LiSi alloys, LiBi alloys, LiCd alloys, AlMg alloys, LiMg alloys, LiSn alloys, LiSb alloys, FeSn alloys, SnSb alloys, SnCu alloys, LiGe alloys, LiPb alloys, oxides thereof, sulfides thereof, phosphides thereof, carbides thereof, nitrides thereof, and any combination thereof. The molecular formula of the anode electroactive compound species may not reflect the empirical formula. Additional examples of anode electroactive species include nitrides, oxides, and carbides of metallic or semi-metallic elements, including Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, Sn, and combinations thereof. In some embodiments, the anode electroactive compound species is silicon. In some embodiments, the electroactive compound species is silicon, and the silicon is in a silicon fiber configuration. In some embodiments, the anode electroactive compound species is Li4Ti5O 12 Examples of salts that can dissolve and generate ionic species that can react to form an anode active electrochemical species include, but are not limited to, K2TiO3, NaKTiO3, Na4Ti5O 12 , LiNO3, LiH2PO4, H2TiO3, H4Ti5O 12, H2TiO5, Co(NO3)2, Ni(NO3)2, Fe(NO3)2, Mn(NO3)2, Al(NO3)3, Li2SO4, CoSO4, NiSO4, FeS O4, MnSO4, Al2(SO4)3, Li(CH3COO), Co(CH3COO)2, Ni(CH3COO)2, Fe(CH3COO)2, Fe3O(CH3C OO)2, Mn(CH3OO)2, AlOH(CH3COO)2, Al3(CH3COO)3, Li(PO4), Co3(PO4)2, Ni3(PO4)2, FePO 4, Mn3(PO4)2, AlPO4, PdSO4, Pd(NO3)2, Pd(CH3COO)2, PtSO4, Pt(NO3)2, Pt(CH3COO)2, Pt( SO4)3, Bi(NO3)3, Bi(CH3OO)3, Ti(SO4)2, Ti(NO3)4, Ti(CH3COO)4, SnSO4, Sn(NO3)2, Sn(C H3COO)2, MgSO4, Mg(NO3)2, Mg(CH3COO)2, W(SO4)5, W(NO3)6, W(CH3COO)4, Ge(SO4)2, Ge(N O3)4, Ge(CH3COO)4, PbSO4, Pb(NO3)2, Pb(CH3COO)2, Zr(SO4)2, Zr(NO3)4, Zr(CH3COO)4, M Includes o(SO4)2, Mo(CH3COO)4, Mg(NO3)2, Mg(CH3COO)2, Ca(NO3)2, Ca(CH3COO)2, and their hydrates. In some embodiments, the first salt 12 is H2TiO3 and the second salt 14 is Li(CH3COO). In some embodiments, the first salt 12 is H2TiO5 and the second salt 14 is Li2SO4. In some embodiments, the nanoparticles 42 may include two or more electroactive compound species that are anode active compound species. For example, in some embodiments, the nanoparticles may include Li4Ti5O 12 and Si-based compounds.

[0051] In some embodiments, when the nanoparticles 42 include at least one compound having catalytic activity, the at least one salt and optional additional salts may be any combination of salts that dissolve into ionic species that can react to form the catalytically active compound species. The additional reactive species may participate in a reaction to form the catalytically active compound. The additional reactive species may be part of a reaction product of the catalytically active compound. Additional reactive species that may be part of the reaction product include oxygen, sulfur, phosphorus, nitrogen, and any combination thereof. The catalytically active compound may be polymetallic. A polymetallic catalytically active compound has two or more metals. Polymetallic catalysts are of interest due to their high catalytic activity. Polymetallic catalysts include precious metals and non-precious metals. Precious metal-based catalysts include elements such as Ru, Rh, Pd, Os, Ir, Pt, and Au. Precious metals are expensive because they are rare, but precious metals have high catalytic efficiency. A means of reducing the cost of precious metal-based catalysts is to increase the surface area / volume ratio of nanoparticles that include catalytically active compounds (e.g., make the nanoparticles smaller). A non-precious metal-based catalyst can include, for example, one or more of Cr, Mn, Fe, Co, Ni, Cu, Zn, or any transition metal, lanthanide, or actinide element that is not a precious metal. A multi-metal catalyst can include one or more precious metals, one or more non-precious metals, or a mixture of precious and non-precious metals. In some embodiments, the nanoparticles 42 include hybrids of catalytically active compounds based on precious and non-precious metals. Hybrids of precious and non-precious metal-based catalysts can be used to reduce costs. The catalytically active compound species of the present disclosure may be polymetallic compounds. The molecular formulas of the catalytically active compound species may not reflect empirical (empirical) formulas. Examples of catalytically active multimetallic compounds include PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, PdCuCe, oxides thereof, sulfides thereof, and phosphides thereof. A catalytically active compound may contain only a single metal.The catalytically active compound species of the present disclosure may contain only a single metal. Non-limiting examples of catalytically active compounds containing a single metal include ZnO, ZnP, Ni2P, NiS, NiCo, NiCu, ZnO, NiO, Cu, AuPt, AuPd, TiO2, and NiO. In some embodiments, the catalytically active compound species is TiO2, NiCo, NiCu, ZnO, NiO, Cu, AuPt, AuPd. Examples of salts that may dissolve into ionic species that can react to form catalytically active compound species include, but are not limited to, TiCl3, Ti(CH3COO)2, TiOSO4, Ti(NO3)4, (NH4)AuCl4, NaAuBr, HAuCl4, KCl, KAuCl4, Na2PdCl4, K2PdBr4, PdCl6, K2PdCl6, (NH4)2PdCl4, K2PdCl4, Na2PtCl4, K2PtBr4, PtCl6, K2PtCl4, (NH4)2PtCl4, K2Pt(NO2)4, KAg(CN)2, KCu, Ni(NO3)2, Mg(NO3)2, NiCl2, PdCl2, Ni(CH3COO)2, NiBr2, NiI2, NiSO4, Pb(CH3COO)2, SeCl2, Se(CH3COO O)2, SeBr4, ZnSO4, Zn(CH3COO)2, Zn(NO3)2, ZnCl2, FeCl2, FeSO4, Fe(NO3)2, RuCl3, Ru(NO3)3, RhCl3 , Rh(NO3)3, IrCl4, Ir2(SO4)3, CuCl2, Cu(NO3)2, CuSO4, Cu(CH3COO)2, SnCl4, Sn(CH3COO)2, SnSO4, Sn (NO3)4, AlCl3, Al2(SO4)3, Al(NO3)3, MgCl2, MgSO4, CoCl2, Co(CH3COO)2, CoSO4, Co(NO3)2, Mn(NO3)2, LiNO3, LiH2PO4, Fe(CH3COO)2, Li2SO4, MnSO4, Al(OCH3)3, Al(CH3COO)3, and any combination thereof. In some embodiments, one or more organic precursors containing the metal of interest can be used. For example, titanium isopropoxide, Ti[OCH(CH3)2]4, may be used as a precursor from the catalyst TiO2.In some embodiments, the first salt 12 is NiCl2, Ni(CH3COO)2, ZnSO4, Zn(CH3COO)2, KCl, or KAuCl4. In some embodiments, the second salt 14 is CoCl2, Co(CH3COO)2, CuCl2, Cu(NO3)2, PdCl6, K2PdCl6, Na2PtCl4, or K2PtBr4.

[0052] In some embodiments, additional reagents can be added to the solution 20. Examples of additional reagents include dopants, stabilizing reagents, and reducing reagents. Examples of reducing reagents include, but are not limited to, tetrabutylammonium borohydride, tetraethylammonium borohydride, tetramethylammonium borohydride, sodium borohydride, sodium triacetoxyborohydride, sodium cyanoborohydride, sodium dihydrogen dihydrido(2-methoxyethoxy)aluminate, potassium borohydride, potassium triethylborohydride, aluminum borohydride, zinc borohydride, ammonium borohydride, lithium aluminum hydride, and hydrazine. Examples of dopants include, but are not limited to, binary heteroatoms, ternary heteroatoms, alkali metals, transition metals, carbon powder, and combinations thereof. Examples of stabilizing reagents include, but are not limited to, SiO2 particles, detergents, and organic ligands. In some embodiments, the organic ligands may be bound to the metal in the catalytically active compound species.

[0053] The sacrificial polymer 16 is generally selected to be at least partially degradable. Examples of suitable degradative processes include, for example, thermal decomposition, thermal oxidation, enzymatic digestion, thermomechanical decomposition, chemical decomposition, photodecomposition, and any combination thereof. Examples of sacrificial polymers include polyhydrocarbons including polyethylene, polypropylene, polystyrene, polyacetylene, and combinations thereof; halopolyhydrocarbons including polyvinyl chloride, polyvinylidene fluoride, polytetrafluoroethylene, and combinations thereof; polyamides including nylon-6, nylon-6,6, nylon-6,10, nylon-11, nylon-12, para-aramid, carbamide-methanal, melamine-methanal, and combinations thereof; polysulfones including poly(arylene sulfone), poly(bisphenol A sulfone), polyether sulfone, polyphenylene sulfone, polysulfone, and combinations thereof; polyethylene glycol, polyether ether ketone, poly(ethylene) oxide, polyvinyl butyral, polycaprolactone, and combinations thereof. Examples of suitable polymers include polyethers including combinations thereof; polyesters including polyethylene terephthalate, polyesters including polyethylene terephthalate, poly(glycolic acid), poly-L-lactic acid, polydioxanone, and combinations thereof; polyamines including polyaniline; polyalcohols including fluoropolyalcohols; polyurethanes; polyacrylates including poly(methyl methacrylate) and polymethyl methacrylate; polycarbonates; polyaromatics including polyethylenedioxythiophene, polyisothianaptene, polypyrrole, and combinations thereof; photosensitive polymers; other polymers including polyvinylpyrrolidone, polyvinyl acetate, cellulose acetate, and polyacrylonitrile; copolymers thereof; block polymers thereof; and combinations thereof. In some embodiments, the sacrificial polymer 16 is or includes a copolymer of styrene butadiene. In some embodiments, the sacrificial polymer 16 is or includes polyvinylpyrrolidone.In some embodiments, the sacrificial polymer 16 is or includes a terpolymer of nylon-6, nylon-6,6, and nylon-6,10. The terpolymer may include, for example, 40 wt% to 50 wt% (e.g., 45 wt%) nylon-6, 15 wt% to 25 wt% (e.g., 20 wt%) nylon-6,6, and 20 wt% to 30 wt% (e.g., 25 wt%) nylon-6,10. In some embodiments, the sacrificial polymer 16 is or includes polyvinyl alcohol. In some embodiments, the sacrificial polymer 16 is or includes polyethylene glycol. The sacrificial polymer 16 may have a variety of topologies, including linear and branched. In some embodiments, multiple sacrificial polymers may be used.

[0054] The molecular weight of the sacrificial polymer 16 can be selected to be compatible with the electrospinning process 2. Generally, higher molecular weight polymers are associated with increased chain entanglement, which may result in a solution 20 having a higher viscosity than a solution 20 containing a lower molecular weight polymer. The viscosity of the solution 20 imposed for electrospinning affects fiber formation. For example, a solution with low viscosity may result in discontinuous fiber formation or electrospraying. A solution with too high a viscosity may result in clogging of the electrospinning machine and / or beading and discontinuous fiber formation. Depending on the polymer (chemical structure and molecular weight) selected, a solution suitable for electrospinning may have a viscosity between 20 cP and 1000 cP measured at room temperature. Viscosity may be measured using a viscometer (e.g., Brookfield LV DV-I Prime Viscometer available from AMETEK Brookfield, Middleboro, Massachusetts) at a set temperature, e.g., 25°C. In some embodiments, the solution 20 has a viscosity of 20 cP or more, 50 cP or more, 100 cP or more, 200 cP or more, or 500 cP or more. The solution may have a viscosity of 1000 cP or less, 800 cP or less, or 600 cP or less.

[0055] Additionally, the molecular weight of the sacrificial polymer 16 can affect the average diameter of the fibers. Generally, higher molecular weight polymers result in fibers having a larger average diameter than fibers formed with lower molecular weight polymers.

[0056] In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is 15,000 g / mol or more, 25,000 g / mol or more, 50,000 g / mol or more, 100,000 g / mol or more, 250,000 g / mol or more, 500,000 g / mol or more, 750,000 g / mol or more, 1,000,000 g / mol or more, or 1,500,000 g / mol or more. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is 25,000 g / mol or less, 50,000 g / mol or less, 100,000 g / mol or less, 250,000 g / mol or less, 500,000 g / mol or less, 1,000,000 g / mol or less, or 1,500,000 g / mol or less. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is between 15,000 g / mol and 1,500,000 g / mol, between 15,000 g / mol and 1,000,000 g / mol, between 15,000 g / mol and 500,000 g / mol, between 15,000 g / mol and 250,000 g / mol, between 15,000 g / mol and 100,000 g / mol, between 15,000 g / mol and 50,000 g / mol, or between 15,000 g / mol and 25,000 g / mol. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is between 25,000 g / mol and 1,500,000 g / mol, between 25,000 g / mol and 1,000,000 g / mol, between 25,000 g / mol and 500,000 g / mol, between 25,000 g / mol and 250,000 g / mol, between 25,000 g / mol and 100,000 g / mol, or between 25,000 g / mol and 50,000 g / mol. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is between 50,000 g / mol and 1,500,000 g / mol, between 50,000 g / mol and 1,000,000 g / mol, between 50,000 g / mol and 500,000 g / mol, between 50,000 g / mol and 250,000 g / mol, or between 50,000 g / mol and 100,000 g / mol.In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is between 100,000 g / mol and 1,500,000 g / mol, between 100,000 g / mol and 1,000,000 g / mol, between 100,000 g / mol and 500,000 g / mol, or between 100,000 g / mol and 250,000 g / mol. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is between 250,000 g / mol and 1,500,000 g / mol, between 250,000 g / mol and 1,000,000 g / mol, or between 250,000 g / mol and 500,000 g / mol. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is from 500,000 g / mol to 1,500,000 g / mol, or from 500,000 g / mol to 1,000,000 g / mol. In some embodiments, the weight average molecular weight of the sacrificial polymer 16 is from 1,000,000 g / mol to 1,500,000 g / mol. In some embodiments, multiple sacrificial polymers may be used, and different sacrificial polymers may have different weight average molecular weights.

[0057] The dispersity of the molecular weight of the sacrificial polymer 16 can affect the properties of the fiber 36. The dispersity of the molecular weight can be quantified as the dispersity (DM). DM is the distribution of the individual molecular weights of the polymer. DM is calculated as the mass average molecular weight (Mw) divided by the number average molecular weight (Mn). Mw and Mn can be determined using various methods such as viscosity measurement, size exclusion chromatography, and mass spectrometry. In general, a small DM is preferred. Electrospinning a polymer with a large DM may result in unstable fiber average diameter and droplet formation. While there is no desirable lower limit, in practice the DM of the sacrificial polymer 16 may be 1.0 or more, 1.1 or more, 1.2 or more, 1.3 or more, 1.4 or more, or 1.8 or more. In some embodiments, the DM of the sacrificial polymer 16 may be 2.0 or less, 1.8 or less, 1.4 or less, 1.3 or less, 1.2 or less, or 1.1 or less. In some embodiments, the DM of the sacrificial polymer 16 is 1.0 to 2.0, 1.0 to 1.8, 1.0 to 1.4, 1.0 to 1.3, 1.0 to 1.2, or 1.0 to 1.1. In some embodiments, the DM of the sacrificial polymer 16 is 1.1 to 2.0, 1.1 to 1.8, 1.1 to 1.4, 1.1 to 1.3, or 1.1 to 1.2. In some embodiments, the DM of the sacrificial polymer 16 is 1.2 to 2.0, 1.2 to 1.8, 1.2 to 1.4, or 1.2 to 1.3. In some embodiments, the DM of the sacrificial polymer 16 is 1.3 to 2.0, 1.3 to 1.8, or 1.3 to 1.4. In some embodiments, the DM of the sacrificial polymer 16 is 1.4 to 2.0, or 1.4 to 1.8. In some embodiments, the DM of the sacrificial polymer 16 is 1.8 to 2.0. In some embodiments, multiple sacrificial polymers may be used, and different sacrificial polymers may have different DM values.

[0058] The amount of sacrificial polymer 16 relative to the amount of total salts present in solution 20 can affect the properties of electrospun fibers 36 and nanoparticles 42. The term "total salts" includes the amount of at least one salt and any additional salts that may be present in solution 20. In some embodiments, the weight % of total salt relative to the weight % of sacrificial polymer 16 is 1 part or more, 2 parts or more, 3 parts or more, 4 parts or more, 5 parts or more, 6 parts or more, 7 parts or more, 8 parts or more, or 9 parts or more of total salt per part sacrificial polymer. In some embodiments, the weight % of total salt relative to the weight % of sacrificial polymer 16 is 10 parts or less, 9 parts or less, 8 parts or less, 7 parts or less, 6 parts or less, 5 parts or less, 4 parts or less, 3 parts or less, or 2 parts or less of total salt per part sacrificial polymer. In some embodiments, the weight percent of total salt to the weight percent of sacrificial polymer 16 is between 1:6 and 2:1, between 1:3 and 5:3, between 2:3 and 5:3, between 2:3 and 4:3, or between 1:3 and 4:3.

[0059] The solvent 26 is generally selected to allow at least one salt 12 and any additional salts to dissociate into their respective ionic species and dissolve the sacrificial polymer 16. Additionally, the solvent 26 is generally selected to be compatible with electrospinning. Thus, the solvent 26 can be selected to have a suitable viscosity for electrospinning the solution 20 by dissolving the sacrificial polymer. The solvent may include one or more protic solvents, aprotic solvents, hydrophobic solvents, hydrophilic solvents, and any combination thereof. Examples of suitable solvents include, but are not limited to, dimethylformamide, isopropanol, ethanol, ether, acetone, carbon tetrachloride, anisole, acetic acid, benzene, dioxane, petroleum ether, acetonitrile, hexane, pyridine, ethyl acetate, cyclohexane, dimethylsulfoxide, 1,2-dichloroethane, chloroform, xylene, methanol, dichloromethane, tetrahydrofuran, acetonitrile, acetone, N-methyl-2-pyrrolidone, water, benzyl alcohol, toluene, and any combination thereof. The solvent may be aqueous. The pH of the solvent may be adjusted to increase the solubility of the salt and the polymer. The pH can be adjusted using an organic acid or base, or an inorganic acid or base. In some embodiments, the solvent is or includes a mixture of isopropanol and dimethylformamide. In some embodiments, the solvent is or includes ethanol. In some embodiments, the solvent is or includes acetone.

[0060] This solution 20 is subjected to electrospinning (arrow 2 in FIG. 1) to produce a sacrificial nonwoven material 30. Electrospinning is an electrohydrodynamic process used in fine fiber production. In general, electrospinning is a process in which a solution is electrically charged to form a jet, and then the jet is stretched to form fibers. Depending on the parameters, the electrospinning process can form one long fiber or many short fibers. The solution and processing parameters of the electrospinning method can be adjusted to obtain the appropriate average diameter and composition of the fibers. Solution parameters include the viscosity of the solution, the polymer concentration, and the molecular weight of the sacrificial polymer. Processing parameters include the conductivity, surface tension, voltage, tip-to-collector distance, feed rate, collector type, collector movement, humidity, pressure, and temperature. Processing parameters depend on the fiber-forming polymer and the solvent or solvents in the solution 20. The applied voltage can affect the fiber properties. Electrospinning conditions typically include voltages between 4 kV and 30 kV. The target-to-collector distance can affect the fiber properties. Electrospinning conditions typically have a target-to-collector distance of 2 cm to 39 cm. In some embodiments, the sacrificial nonwoven material is deposited on a rotating cylindrical collector. In some embodiments, the sacrificial nonwoven material is deposited on a stationary collector. In some embodiments, the solution 20 can be subjected to conventional electrospinning, coaxial electrospinning, emulsion electrospinning, or molten electrospinning.

[0061] The weight percent of total solids in solution 20 can affect the properties of the sacrificial nonwoven material 30. The total solids include the first salt, any additional salts, any additional components, and the sacrificial polymer. In some embodiments, the weight percent of total solids in solution 20 is 5% or more, 10% or more, 15% or more, 20% or more, 30% or more, or 40% or more. In some embodiments, the weight percent of total solids in solution is 50% or less, 40% or less, 30% or less, 20% or less, 15% or less, 10% or less, or 5% or less. In some embodiments, the weight percent of total solids is between 5% and 50%, between 5% and 40%, between 5% and 30%, between 5% and 20%, between 5% and 15%, between 5% and 10%, between 10% and 50%, between 10% and 40%, between 10% and 30%, between 10% and 20%, between 10% and 15%, between 15% and 50%, between 15% and 40%, between 15% and 30%, between 15% and 20%, between 20% and 50%, between 20% and 40%, between 20% and 30%, between 30% and 50%, between 30% and 40%, between 40% and 50%, between 10% and 20%, between 20% and 30%. In some embodiments, when the sacrificial polymer is nylon, the weight percent of total solids in the solution is between 10% and 25%. In some embodiments, when the sacrificial polymer is cellulose acetate, the weight percent of total solids in the solution is at least 20% and 30%.

[0062] The sacrificial nonwoven material 30 includes fibers 36. The fibers 36 may be a single fiber or multiple fibers. The sacrificial polymer 16 is the fiber-forming component of the fibers 36. Thus, the fibers 36 include the sacrificial polymer 16, and the first ionic species 22 and the second ionic species 24. The first ionic species 22 and the second ionic species 24 attach to the polymer 16 and across the fibers 36. Examples of attachment forces include metal-ligand interactions, electrostatic attraction, π-π stacking, and combinations thereof. In some embodiments, the first ionic species 22 and the second ionic species 24 are uniformly distributed across the fibers 36. Each fiber 36 has an average diameter. The average diameter can be measured using a variety of techniques, including scanning electron microscopy or transmission electron microscopy. In some cases, the fibers can be characterized as nanofibers. However, the fibers of the present disclosure are not necessarily limited to submicron diameter fibers. In some embodiments, the fibers 36 have an average diameter of 5 μm or less, 4 μm or less, 3 μm or less, 2 μm or less, 1.5 μm or less, 1.2 μm or less, 1.0 μm or less, 0.8 μm or less, 0.6 μm or less, 0.4 μm or less, or 0.2 μm or less. In some embodiments, the fibers 36 have an average diameter of 0.1 μm or more, 0.2 μm or more, 0.4 μm or more, 0.5 μm or more, 0.6 μm or more, 0.8 μm or more, 1.0 μm or more, or 1.2 μm or more. In some embodiments, fibers 36 have an average diameter of 0.1 μm to 5 μm, 0.1 μm to 4 μm, 0.1 μm to 3 μm, 0.1 μm to 2 μm, 0.5 μm to 5 μm, 0.5 μm to 4 μm, 0.5 μm to 3 μm, 0.5 μm to 2 μm, 0.8 μm to 5 μm, 0.8 μm to 4 μm, 0.8 μm to 3 μm, 0.8 μm to 2 μm, 1 μm to 5 μm, 1 μm to 4 μm, 1 μm to 3 μm, 0.1 μm to 1.5 μm, 0.2 μm to 1.5 μm, 0.4 μm to 1.5 μm, 0.6 μm to 1.5 μm, 0.8 μm to 1.5 μm, 1.0 μm to 1.5 μm, or 1.2 μm to 1.5 μm. In some embodiments, the fibers 36 have an average diameter of 0.1 μm to 1.2 μm, 0.2 μm to 1.2 μm, 0.4 μm to 1.2 μm, 0.6 μm to 1.2 μm, 0.8 μm to 1.2 μm, or 1.0 μm to 1.2 μm.In some embodiments, fibers 36 have an average diameter of 0.1 μm to 1.0 μm, 0.2 μm to 1.0 μm, 0.4 μm to 1.0 μm, 0.6 μm to 1.0 μm, or 0.8 μm to 1.0 μm. In some embodiments, fibers 36 have an average diameter of 0.1 μm to 0.8 μm, 0.2 μm to 0.8 μm, 0.4 μm to 0.8 μm, or 0.6 μm to 0.8 μm.

[0063] In some embodiments, the smaller the average diameter of the fibers 36, the smaller the size of the nanoparticles 42 formed after the decomposition process 3. Generally, fibers with a smaller average diameter are associated with the formation of smaller nanoparticles 42. In some embodiments, the smaller the average diameter of the fibers, the less energy (e.g., thermal energy) required for the decomposition process 3.

[0064] The sacrificial nonwoven material 30 is subjected to a decomposition process (arrows 3) to obtain a blend 40. The blend 40 includes a plurality of nanoparticles 42. The blend 40 may include decomposed or partially decomposed fibers 46. The decomposition process 3 may promote a chemical reaction between at least the first ionic species 22 and the second ionic species 24, resulting in at least one compound species. In some embodiments, additional species may be part of the reaction product. Examples of additional reactive species include oxygen, sulfur, phosphorus, nitrogen, and combinations thereof. The nanoparticles 42 are formed from a plurality of compound species assembled in a crystalline structure. In some embodiments, the compound species are electroactive. Examples of suitable electroactive compound species include LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, and Li(Ni x Al y Co z)O2, where x+y+z=1. In some embodiments, the compound species is catalytically active. Examples of suitable catalytically active compounds include PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, PdCuCe, and oxides, sulfides, and phosphides thereof.

[0065] In some embodiments, the nanoparticles 42 have a narrow particle size distribution. In some embodiments, the nanoparticles 42 have a particle size range of 0.005 μm to 0.5 μm, 0.005 μm to 0.4 μm, 0.005 μm to 0.3 μm, 0.005 μm to 0.2 μm, 0.005 μm to 0.1 μm, 0.005 μm to 0.05 μm, 0.005 μm to 0.05 μm, 0.005 μm to 0.04 μm, 0.005 μm to 0.03 μm, 0.005 μm to 0.02 μm, or 0.005 μm to 0.01 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.01 μm to 0.5 μm, 0.01 μm to 0.4 μm, 0.01 μm to 0.3 μm, 0.01 μm to 0.2 μm, 0.01 μm to 0.1 μm, 0.01 μm to 0.05 μm, 0.01 μm to 0.04 μm, 0.01 μm to 0.03 μm, or 0.01 μm to 0.02 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.02 μm to 0.5 μm, 0.02 μm to 0.4 μm, 0.02 μm to 0.3 μm, 0.02 μm to 0.2 μm, 0.02 μm to 0.1 μm, 0.02 μm to 0.05 μm, 0.02 μm to 0.04 μm, or 0.02 μm to 0.03 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.03 μm to 0.5 μm, 0.03 μm to 0.4 μm, 0.03 μm to 0.3 μm, 0.03 μm to 0.2 μm, 0.03 μm to 0.1 μm, 0.03 μm to 0.05 μm, or 0.03 μm to 0.04 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.04 μm to 0.5 μm, 0.04 μm to 0.4 μm, 0.04 μm to 0.3 μm, 0.04 μm to 0.2 μm, 0.04 μm to 0.1 μm, or 0.04 μm to 0.05 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.05 μm to 0.5 μm, 0.05 μm to 0.4 μm, 0.05 μm to 0.3 μm, 0.05 μm to 0.2 μm, or 0.05 μm to 0.1 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.1 μm to 0.5 μm, 0.1 μm to 0.4 μm, 0.1 μm to 0.3 μm, or 0.1 μm to 0.2 μm. In some embodiments, the nanoparticles 42 have a particle size range of 0.2 μm to 0.5 μm, 0.2 μm to 0.4 μm, or 0.2 μm to 0.3 μm.In some embodiments, the nanoparticles 42 have a size range of 0.3 μm to 0.5 μm or 0.3 μm to 0.4 μm, hi some embodiments, the nanoparticles 42 have a size range of 0.4 μm to 0.5 μm.

[0066] The decomposition process 3 is generally selected to decompose at least a portion of the sacrificial nonwoven material 30. The sacrificial nonwoven material 30 includes fibers 36. The fibers include a first ionic species 22 and a second ionic species 24. The decomposition process creates a mass difference between the sacrificial nonwoven material 30 and the blend 40. The blend 40 includes a plurality of nanoparticles. The blend 40 may include decomposed or partially decomposed fibers 36. The degree of decomposition can be characterized as the difference in mass between the sacrificial nonwoven material 30 and the blend 40. Decomposition of the sacrificial polymer may contribute to the mass change. Decomposition of the first salt and the second salt may contribute to the mass change. The degree of decomposition can be measured as the quotient of the initial total mass of the sacrificial polymer and salt added to the solution 20 and the mass of the blend 40. In some embodiments, the decomposition process 3 decomposes 25% or more, 50% or more, or 75% or more of the sacrificial nonwoven material 30. In some embodiments, the decomposition process 3 decomposes 99% or less, 95% or less, 90% or less, 75% or less, 50% or less, or 25% or less of the nonwoven material 30. In some embodiments, the decomposition process 3 may decompose 25%-99%, 25%-95%, 25%-90%, 25%-75%, 25%-50%, or 25%-50% of the sacrificial nonwoven material 30. In some embodiments, the decomposition process 3 may decompose 50%-99%, 50%-95%, 50%-90%, or 50% of the sacrificial nonwoven material 30. In some embodiments, the decomposition process 3 may decompose 75%-99%, 75%-95%, or 75%-90% of the sacrificial nonwoven material 30. In some embodiments, the decomposition process 3 may decompose 90%-99%, or 90%-95% of the sacrificial nonwoven material 30. In some embodiments, the decomposition process 3 may decompose 95%-99% of the sacrificial nonwoven material 30.

[0067] The decomposition treatment 3 is generally selected to decompose at least a portion of the fibers 36 by decomposing at least a portion of the sacrificial polymer 16, resulting in a decomposed fiber 46. Examples of suitable decomposition treatments include pyrolysis, thermo-oxidation, enzymatic digestion, thermo-mechanical decomposition, chemical decomposition, photolysis, and any combination thereof. In some embodiments, the blend 40 is subjected to a post-decomposition treatment. One example of a post-decomposition treatment is sieving the blend 40 to separate at least a portion of the nanoparticles from the decomposed fibers 36. In some embodiments, nanoparticles of a particular size range can be separated from the blend 40 via filtering.

[0068] In some embodiments, the decomposition process 3 includes pyrolysis in the form of pyrolysis. Pyrolysis is the thermal decomposition of materials at high temperatures in an inert atmosphere (e.g., little to no oxygen). In some embodiments, a gas such as oxygen may be added during pyrolysis to promote combustion of the fibers 36. In some embodiments, the decomposition process 3 includes pyrolysis at temperatures of 400° C. or more, 500° C. or more, at least 600° C. or more, at least 700° C. or more, or 800° C. or more. In some embodiments, the decomposition process 3 includes pyrolysis at temperatures of 500° C. or less, 600° C. or less, 700° C. or less, 800° C. or less, 900° C. or less, 1000° C. or less, or 1100° C. or less. In some embodiments, the decomposition treatment 3 comprises pyrolysis at a temperature effective to decompose the sacrificial polymer to a desired extent, such as 400° C. to 1100° C., 400° C. to 1000° C., 400° C. to 900° C., 400° C. to 800° C., 400° C. to 700° C., 400° C. to 600° C., 400° C. to 700° C., 500° C. to 1100° C., 500° C. to 1000° C., 500° C. to 900° C., 500° C. to 800° C., 500° C. to 700° C., or 500° C. to 600° C. In some embodiments, the temperature of pyrolysis can be varied throughout the pyrolysis process.

[0069] In some embodiments, the pyrolysis process forms an artificial solid electrolyte interface in the form of a carbonaceous layer around the individual nanoparticles. Transmission electron microscopy can be used to measure the thickness of the carbonaceous layer. In some embodiments, the carbonaceous layer is 10 nm or less, 5 nm or less, 2 nm or less, or 1 nm or less in thickness. In some embodiments, the carbonaceous layer is 1 nm or more, 2 nm or more, or 5 nm or more in thickness. In some embodiments, the carbonaceous layer is 1 nm to 10 nm, 1 nm to 5 nm, or 1 nm to 2 nm in thickness. In some embodiments, the carbonaceous layer is 2 nm to 10 nm, or 2 nm to 5 nm in thickness. In some embodiments, the carbonaceous layer is 5 nm to 10 nm in thickness. The carbonaceous layer may not impede the diffusion of lithium ions into and out of the crystal lattice of the electroactive nanoparticles. In some embodiments, the artificial solid electrolyte interface can improve battery life by reducing capacity fade.

[0070] In some embodiments, pyrolysis includes carbonization of the fibers 36, resulting in decomposed fibers 46 that are elemental carbon. In some embodiments, the fibers 36 are partially pyrolyzed, resulting in decomposed fibers 46 that include carbon, the sacrificial polymer 16, and low molecular weight polymers formed by severing various bonds in the sacrificial polymer 16 during the pyrolysis process. Incomplete pyrolysis may be beneficial because the remaining polymer and low molecular weight polymer may act as a passive layer for an electrode assembly. Incomplete pyrolysis of the fibers 36 may be beneficial because the remaining polymer and low molecular weight polymer may act as a support for a catalytic assembly.

[0071] Without wishing to be bound by theory, it is believed that the nanoscale anisotropy of the fibers produced by the disclosed method allows for the conversion of ionic species to electroactive nanoparticles at pyrolysis temperatures as low as 550° C., producing highly crystalline nanoparticles (see, e.g., FIG. 7). In contrast, many other protocols for producing electroactive materials require temperatures greater than 700° C. The reduced pyrolysis temperature compared to other protocols can lead to energy and economic savings. According to an embodiment, the disclosed electroactive nanoparticles are highly stable. For example, in some embodiments, the disclosed cathodic electroactive nanoparticles are stable after 100 or more charge-discharge cycles. The disclosed method for making nanoparticles may also allow for a reduction in the number of steps used to apply an artificial solid electrolyte interface to the nanoparticles. For example, many protocols apply an artificial solid electrolyte interface as a separate post-processing step using atomic layer deposition, molecular layer deposition, chemical vapor deposition, or sol-gel processes. In contrast, in some embodiments of the present disclosure, an artificial solid electrolyte interface can be formed in situ from a thin carbon layer on the nanoparticles by pyrolysis processing.

[0072] The process of the present disclosure may be used to prepare a composition. According to one embodiment, the composition includes an electrospun nonwoven layer. The electrospun nonwoven layer may include a substrate and fibers deposited on the substrate by electrospinning. The fibers may be comprised of a polymer and a plurality of nanoparticles dispersed on the polymer and distributed throughout the fibers. The plurality of nanoparticles may have a particle size range of 0.01 μm to 0.5 μm. Each nanoparticle may include a plurality of at least one chemical species. In some embodiments, the composition is used to manufacture an electrode assembly.

[0073] According to one embodiment, the composition includes a substrate and two fiber layers deposited on the substrate by electrospinning. The fiber layers may include fibers made of a polymer and a plurality of nanoparticles dispersed on the polymer and distributed throughout the fibers. Each fiber layer may have a different density, with one layer having a density at least 1.1 times higher than the other layer. In some embodiments, the layer having the higher density is deposited first adjacent to the substrate and the layer having the lower density is deposited later on the first layer. The plurality of nanoparticles may have a particle size range of 0.01 μm to 0.5 μm. Each nanoparticle may include a plurality of at least one compound. In some embodiments, the composition is used to fabricate an electrode assembly.

[0074] According to one embodiment, the composition includes a substrate and an electrospun nonwoven layer including a fiber layer deposited on the substrate by electrospinning. The fiber layer may include the fibers, each fiber having a fiber diameter of 0.1 μm to 5 μm. The fibers may include a polymer and a plurality of nanoparticles dispersed on the polymer and distributed throughout the fibers. The plurality of nanoparticles may have a particle size range of 0.01 μm to 0.5 μm. Each nanoparticle may include a plurality of at least one compound. In some embodiments, the composition is used to fabricate an electrode assembly.

[0075] FIG. 2 is a schematic diagram of a process used to manufacture an electrode assembly 60. In some embodiments, the electrode assembly 60 is a cathode assembly. In some embodiments, the electrode assembly 60 is an anode assembly. The solution 50 is spun (e.g., electrospun) 4 onto a substrate 64 producing a nonwoven layer 62. The solution 50 includes nanoparticles 42 containing electroactive compound species, a conductive material 54, and a binder polymer 56, all dissolved in a solvent 52. The electroactive compound can include any electroactive compound species or combination of electroactive compound species. Examples of cathode electroactive compound species include LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Coz )O2, and Li(Ni x Al y Co z )O2, where x+y+z=1. Examples of anode active electroactive compound species include Co3O4, Cu2O, Li4Ti5O 12 (lithium titanate), SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO and carbides thereof, and combinations thereof. Further examples of anode electroactive species include LiAl alloys, LiSi alloys, LiBi alloys, LiCd alloys, AlMg alloys, LiMg alloys, LiSn alloys, LiSb alloys, FeSn alloys, SnSb alloys, SnCu alloys, LiGe alloys, LiPb alloys, oxides thereof, sulfides thereof, phosphides thereof, carbides thereof, nitrides thereof, and combinations thereof. Further examples of anode active electroactive species include nitrides, oxides, carbides of metallic or semi-metallic elements, including Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, Sn, and combinations thereof. In some embodiments, the nanoparticles 42 may have been prepared using the process described with reference to FIG. 1.

[0076] Solution 50 is subjected to electrospinning 4 to produce nonwoven layer 62. Nonwoven layer 62 includes fibers 66. Binder polymer 56 is a fiber-forming component of fibers 66. Thus, fibers 66 include binder polymer 56. Conductive material 54 and nanoparticles 42 are bound to binder polymer 56 and distributed along fibers 66. In some embodiments, conductive material 54 and nanoparticles 42 are uniformly distributed along fibers 66. In some embodiments, fibers 66 are single fibers. In some embodiments, fibers 66 are multiple fibers. Any of the electrospinning methods discussed with reference to the process described in FIG. 1 may be used.

[0077] In some embodiments, the nanoparticles 42 have a narrow size distribution. The nanoparticles may have any of the size ranges disclosed elsewhere herein. The solvent 52 can be selected to allow for dispersion, preferably uniform dispersion, of the nanoparticles 42 and the conductive material 54, and dissolution of the binder polymer 56. The solvent 52 can be selected to minimize dissolution of the nanoparticles 42 into the component ions. The solvent 52 is preferably selected to be compatible with the electrospinning process. Suitable solvents include protic solvents, aprotic solvents, hydrophobic solvents, hydrophilic solvents, and any combination thereof. Examples of suitable solvents include, but are not limited to, dimethylformamide, isopropanol, ethanol, ether, acetone, carbon tetrachloride, anisole, acetic acid, benzene, dioxane, petroleum, ether, acetonitrile, hexane, pyridine, ethyl acetate, cyclohexane, dimethylsulfoxide, 1,2-dichloroethane, chloroform, xylene, methanol, dichloromethane, tetrahydrofuran, acetonitrile, acetone, N-methyl-2-pyrrolidone, water, benzyl alcohol, toluene, and any combination thereof. The solvent may be aqueous. The pH of the solvent may be adjusted to reduce the solubility of the nanoparticles. The pH may be adjusted to increase the solubility of the binder polymer. The pH may be adjusted using an organic acid or base, or an inorganic acid or base.

[0078] The binder polymer 56 is generally selected to bind the nanoparticles 42 and the conductive material 54. The binder polymer itself may be conductive. Examples of binder polymers include polyhydrocarbons, including polyethylene, polypropylene, polystyrene, polyacetylene, and the like; halopolyhydrocarbons, including poly(vinyl chloride), polyvinylidene fluoride, poly(tetrafluoroethylene), and the like; polyamides, such as nylon-6, nylon-6,6, nylon-6,10, nylon-11, nylon-12, para-aramid, carbamide-methanal, melamine-methanal, and the like; polysulfones, such as poly(arylene sulfone), poly(bisphenol A sulfone), polyether sulfone, polyphenylene sulfone, and polysulfone; polyethylene glycol, polyether ether ketone, poly(ethylene) oxide, polyether ether ketone ... Examples of binder polymers include polyethers such as teresulfone; polyesters such as polyethylene terephthalate, poly(glycolic acid), poly-L-lactic acid, polydioxanone; polyamines such as polyaniline; polyalcohols such as fluorinated polyalcohols; polyurethanes; polycarbonates; polyaromatics such as polyethylenedioxythiophene, polyisothianaptene, polypyrrole, poly(3-hexylthiophene); polyimides; photosensitive polymers; other polymers including polyacrylates, polyvinylpyrrolidone; and block polymers, such as copolymers of styrene butadiene; copolymers thereof; block polymers thereof; and combinations thereof. In some embodiments, the binder polymer 56 is a styrene butadiene copolymer. In some embodiments, the binder polymer 56 is polyvinylidene fluoride.

[0079] In the electrode assembly 60, the substrate 64 can be selected as a current collector. The electrode assembly can be compatible with materials and types of current collectors known in the art. For example, the substrate 64 can include one or more materials capable of collecting current, such as Cu, Al, Ni, Ti, Pt, stainless steel, carbon, or any combination thereof. The current collector material can be in the form of a foil, mesh, foam, woven layer, or non-woven layer. In some embodiments, the substrate includes Cu foil, Al foil, Pt foil, or Ni foil. The current collector material can coat the surface of an additional substrate. The current collector can be an artificial double solid-electrolyte interface. In some embodiments, post-electrospinning treatments, such as known mechanical and / or chemical treatments, can be used to bond the non-woven layer 62 to the substrate 64.

[0080] The conductive material 54 may be selected to enhance the electronic and ionic conductivity of the electrode assembly 60. Any suitable conductive material known in the art may be used. Examples of suitable conductive materials include, but are not limited to, carbon powder, carbon fiber, graphite, carbon nanotubes, graphene, graphine, bronze, copper, tungsten, carbon steel, silver, gold, aluminum, zinc, INCONEL (available from American Special Metals, Corp, Miami, Fla.), HASTELLOY (available from Hastelloy International Corporation, Tipton, Ind.), KOVAR (available from CRS Holdings Inc., Oklahoma City, Okla.), and combinations thereof.

[0081] Without wishing to be bound by theory, it is believed that the electrode assemblies made by the disclosed method result in a nonwoven layer 62 with a large electrode / electrolyte interfacial area that allows for improved electrochemical oxidation and reduction reaction kinetics compared to conventional slurry cast electrodes. Additionally, the use of electrospinning to fabricate the nonwoven layer 62 may allow for tailoring of the interfiber void volume that allows for better electrolyte penetration into the electrode. Additionally, the sub-micrometer fibers 66 may allow for dispersion of the nanoparticles 42 with minimal agglomeration. The sub-micrometer fibers 66 may also have a high nanoparticle content that may allow for short lithium ion transport pathways. Additionally, the disclosed method may be broadly adaptable to a wide selection of nanoparticle species and polymer combinations.

[0082] The electrode assembly can be used in batteries. Battery types include, but are not limited to, alkaline, aluminum-air, atomic, bunsen, grove, mercury, molten salt, nickel oxyhydroxide, organic radical, silver oxide, zinc oxide, zinc-carbon, zinc-chloride, aluminum-ion, calcium, vanadium redox, zinc-bromine, zinc-cerium, lead-acid, lithium-ion, lithium metal, magnesium-ion, metal-air, nickel-cadmium, nickel-hydrogen, nickel-iron, nickel-hydrogen, polymer-based, polysulfide-bromide, potassium-ion, zinc-ion. In some embodiments, the cathode assembly is used in lithium-ion batteries. Lithium-ion batteries include, but are not limited to, lithium-cobalt oxide, lithium-silicon, lithium-manganese oxide, lithium-polymer, lithium-nickel-manganese-cobalt oxide, lithium-nickel-cobalt-aluminum oxide, lithium-sulfur, lithium-titanate, and lithium-ceramic batteries.

[0083] In some embodiments, the battery is a lithium ion battery. Examples of cathode electroactive compound species that may be used in the lithium ion battery cathode assembly are discussed elsewhere herein. Examples of anode electroactive compound species that may be used in the lithium ion battery anode assembly are discussed elsewhere herein. In some embodiments, at least a portion of the cathode assembly and / or anode assembly is obtained as described in the process with reference to FIG. 2.

[0084] FIG. 4A shows a typical lithium-ion battery 100. The battery 100 has a cathode 120, an anode 122, an electrolyte 104, and a separator 106. The electrolyte 104 can be any suitable electrolyte, such as a polymer electrolyte, a liquid electrolyte, or the like. Examples of electrolytes include solutions of LiPF6 (lithium hexafluorophosphate), LiBF4 (lithium tetrafluoroborate), LiClO4 (lithium perchlorate), and any combination thereof. The electrolyte solution can be prepared in one or more organic solvents. Examples of organic solvents include carbonate organic solvents including dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, propylene carbonate; and other organic solvents including acetonitrile; and any combination thereof. Any suitable separator 106 can be used, including, for example, polymeric porous membranes such as polyethylene, polypropylene (CELGARD); modified polymeric membranes with thin oxide coatings of titania (TiO2), zinc oxide (ZnO), silica (SiO2); and hybrid organic-organic assemblies such as those containing SiO2 nanoparticles covalently bonded within a polymer network such as polyurethane, polyacrylate, polyethylene glycol. In some embodiments, multiple separators can be used.

[0085] In some embodiments, the cathode 120 and / or the anode 122 include an electrode assembly 60. The electrode assembly 60 includes a nonwoven layer 62 that is deposited on a substrate 64 (FIG. 4B). In some embodiments, the electrode assembly 60 is included in the cathode 120. In some embodiments, the electrode assembly 60 is included in the anode 122. In some embodiments, the electrode assembly 60 is included in the cathode 120 and the anode 122.

[0086] 3 is a schematic diagram of a process used to manufacture a catalytic mass 600. A solution 500 is spun (e.g., electrospun; arrow 5) onto a substrate 640 producing a nonwoven layer 620. The solution 500 includes nanoparticles 42 and a binder polymer 560 dissolved in a solvent 520. The nanoparticles 42 can include any catalytically active compound species. Examples of catalytically active compound species are described elsewhere herein. In an exemplary embodiment, the nanoparticles 42 may have been prepared using the process described with respect to FIG. 1.

[0087] In some embodiments, the nanoparticles 42 have a narrow size distribution. The nanoparticles 42 may have any size range, as disclosed elsewhere herein.

[0088] Binder polymer 560 is generally selected to bind nanoparticles 42. Binder polymer 560 can be any of the binder polymers described with reference to binder polymer 56.

[0089] Solvent 520 may be selected to dissolve binder polymer 560 while allowing dispersion, preferably uniform dispersion, of nanoparticles 42. Solvent 520 may be selected to reduce or minimize dissolution of nanoparticles 42 in the component ions. Solvent 520 may be any of the solvents described with reference to solvent 52.

[0090] Solution 500 is subjected to electrospinning 5 to produce nonwoven layer 620. Nonwoven layer 620 includes fibers 42. Binder polymer 560 is a fiber-forming component of fibers 660. Thus, fibers 660 include binder polymer 560. Nanoparticles 42 are bound to binder polymer 560 and distributed along fibers 660. In some embodiments, nanoparticles 42 are uniformly distributed along fibers 660. In some embodiments, fibers 660 are single fibers. In some embodiments, fibers 660 are multiple fibers. Any of the electrospinning methods discussed with reference to the process described in FIG. 1 can be used.

[0091] Without wishing to be bound by theory, it is believed that the catalyst assemblies created via the methods of the present disclosure allow for sub-micrometer fibers that minimize agglomeration and allow dispersion of the nanoparticles 42. Minimizing the agglomeration of the nanoparticles may increase the surface area of ​​the nanoparticles and improve the ability of the catalytically active compound species to catalyze a reaction. Additionally, increasing the catalyst surface area may be economical and environmentally friendly since less catalyst is required to carry out the desired reaction. Additionally, in some embodiments, the fibers 660 may provide a support for the catalyst that may allow for greater catalyst turnover and stability.

[0092] In the catalytic assembly 600, the substrate 640 is generally selected to support the nonwoven layer 620. The substrate 640 can provide physical support to the nonwoven layer 620. Substrates that provide physical support include, but are not limited to, metal, paper, plastic, and the like. The substrate can be selected so as not to alter the catalytic activity of the compounds in the nanoparticles. Examples of such substrates that do not affect the reactivity of the catalyst include silicon dioxide, aluminum dioxide, ceramic-containing materials, and the like. The substrate can be selected so as to promote the catalytic activity of the compounds in the nanoparticles. Examples of substrates that may promote the catalytic activity of the compounds in the nanoparticles include, but are not limited to, carbon nanotubes and other carbon structures. The substrate 640 can be single layered or multi-layered. Each layer of the multi-layered substrate can be made of a different material. For example, in the case of a two-layered substrate, the layer in contact with the nonwoven layer 620 can include silicon dioxide, and the layer not in contact with the nonwoven layer can be metal. In some embodiments, the nonwoven layer can be adhered to the substrate 640 using known mechanical and / or chemical methods.

[0093] The catalytic assembly 600 can be used to catalyze reactions. An appropriate amount of the catalytic assembly can be exposed to a reagent to catalyze the chemical conversion of one or more of the reagents. For example, a catalytic assembly 600 including nanoparticles made of PtPdO can be used to catalyze the combustion of methane. In another example, a catalytic assembly 600 including nanoparticles made of NiO can be used to catalyze the coupling reaction of an aldehyde, an amine, and an alkyne to produce propargylamine. In yet another example, a catalytic assembly 600 including nanoparticles made of CuNi, CuCo, or CuFe, or a combination thereof, can be used to catalyze the partial oxidation of propylene to acrolein.

[0094] In some embodiments, the nonwoven layer 620 may be removed from the substrate 640 and used as a catalyst. In this embodiment, the binder polymer provides support for the nanoparticles. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0095] A non-exhaustive list of exemplary aspects is provided below. Any one or more of the features of these aspects can be combined with any one or more features of another example, embodiment, or aspect described herein.

[0096] [Embodiment A. Composition] According to embodiment 1A, a composition comprises an electrospun nonwoven material comprised of fibers having an average diameter of less than 5 μm, a sacrificial polymer present at 40% to 60% by weight of a total weight of the electrospun nonwoven material, and a first ionic species and a second ionic species dispersed on the sacrificial polymer and distributed along the fibers, the first ionic species and the second ionic species being ionic species of at least one salt, the at least one salt being present at 60% or less by weight of total salt, and the weight % of total salt to weight % of the sacrificial polymer is greater than or equal to 1 part by weight of the total salt to 6 parts by weight of the sacrificial polymer.

[0097] Embodiment 2A is the composition of embodiment 1A, wherein the at least one salt comprises NiCl2, Ni(CH3COO)2, ZnSO4, Zn(CH3COO)2, KCl, KAuCl4, CoCl2, Co(CH3COO)2, CuCl2, Cu(NO3)2, PdCl6, K2PdCl6, Na2PtCl4, K2PtBr4, Ni(NO3)2, Co(NO3)2, Mn(NO3)2, Al(NO3)3, Fe(NO3)2, LiNO3, LiH2PO4, Fe(CH3COO)2, NiSO4, CoSO4, Li2SO4, MnSO4, FeSO4, Al2(SO4)3, Al(OCH3)3, Al(CH3COO)3, or combinations thereof.

[0098] Embodiment 3A is the composition of any one of the preceding embodiments, wherein the sacrificial polymer is polyvinylpyrrolidone, polyethylene glycol, nylon, polyurethane, polyvinyl alcohol, polyvinyl acetate, polyacrylonitrile, polyacrylate, or a combination thereof. In some embodiments, the sacrificial polymer is one or more of polyamide, polysulfone, polyether, polyester, polyamine, polyalcohol, polyurethane, polycarbonate, polyaromatics, photopolymer, polyimide, or a combination thereof.

[0099] Embodiment 4A is the composition of any one of the previous embodiments, wherein the weight percent of total salt to the weight percent of sacrificial polymer is 1:6 to 2:1, 1:3 to 5:3, 2:3 to 5:3, 2:3 to 4:3, or 1:3 to 4:3.

[0100] Embodiment 5A is the composition of any one of the previous embodiments, wherein the fibers have an average diameter of 4 μm or less, 3 μm or less, 2 μm or less, 1.5 μm or less, or 1 μm or less.

[0101] Embodiment 6A is a composition of any one of the preceding embodiments, wherein at least one chemical species is electroactive.

[0102] Embodiment 7A is the composition of embodiment 6A, wherein at least one compound species is LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, Li(Ni x Al y Co z )O2, or a combination thereof, where x+y+z=1. In some embodiments, the at least one compound species is Co3O4, Cu2O, Li4Ti5O 12, SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO, and carbides thereof; LiAl alloy, LiSi alloy, LiBi alloy, LiCd alloy, AlMg alloy, LiMg alloy, LiSn alloy, LiSb alloy, FeSn alloy, SnSb alloy, SnCu alloy, LiGe alloy, LiPb alloy, oxides thereof, sulfides thereof, phosphides thereof, carbides thereof, and nitrides thereof; nitrides, oxides, and carbides of Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, and Sn; silicon; or combinations thereof.

[0103] Embodiment 8A is a composition of any one of the preceding embodiments, wherein at least one compound species has catalytic activity.

[0104] Embodiment 9A is the composition of embodiment 8A, wherein at least one compound species comprises PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, TiO2, NiO, or a combination thereof.

[0105] Embodiment 10A is a composition comprising a first plurality of nanoparticles, each nanoparticle comprising a first compound species, and a second plurality of nanoparticles, each nanoparticle comprising a second compound species different from the first compound species, wherein the first and second plurality of nanoparticles have a particle size range of 0.01 μm to 0.5 μm.

[0106] [Embodiment B. Composition] According to embodiment 1B, a composition includes an electrospun nonwoven layer comprising a substrate and fibers deposited on the substrate by electrospinning, the fibers comprising a polymer and a plurality of nanoparticles dispersed on the polymer and distributed throughout the fibers, the plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm, and each nanoparticle comprising a plurality of at least one chemical species.

[0107] Embodiment 2B is the composition of embodiment 1B including a plurality of fibers forming a first fibrous layer.

[0108] Embodiment 3B is a composition according to any one of embodiments 1B-2B, further comprising a second fiber layer comprising second fibers deposited on the first fibers by electrospinning, the second fibers comprising a second polymer and a second plurality of nanoparticles dispersed on the second polymer and distributed throughout the fibers, the second plurality of nanoparticles being between 0.1 μm and 0.5 μm, each nanoparticle comprising a plurality of at least one compound species, and the first fiber layer having a density that is at least 1.1 times the density of the second fiber layer.

[0109] Embodiment 4B is the composition of any one of embodiments 1B-3B, wherein the fibers have an average diameter of 5 μm or less, 4 μm or less, 3 μm or less, 2 μm or less, 1.5 μm or less, 1.0 μm or less, 0.8 μm or less, 0.6 μm or less, 0.4 μm or less, or 0.2 μm or less. In some embodiments, the fibers have an average diameter of at least 0.1 μm, at least 0.2 μm, at least 0.4 μm, at least 0.5 μm, at least 0.6 μm, at least 0.8 μm, at least 1.0 μm, or at least 1.2 μm. In some embodiments, fibers 36 have an average diameter of 0.1 μm to 5 μm, 0.1 μm to 4 μm, 0.1 μm to 3 μm, 0.1 μm to 2 μm, 0.5 μm to 5 μm, 0.5 μm to 4 μm, 0.5 μm to 3 μm, 0.5 μm to 2 μm, 0.8 μm to 5 μm, 0.8 μm to 4 μm, 0.8 μm to 3 μm, 0.8 μm to 2 μm, 1 μm to 5 μm, 1 μm to 4 μm, 1 μm to 3 μm, 0.1 μm to 1.5 μm, 0.2 μm to 1.5 μm, 0.4 μm to 1.5 μm, 0.6 μm to 1.5 μm, 0.8 μm to 1.5 μm, 1.0 μm to 1.5 μm, or 1.2 μm to 1.5 μm.

[0110] Embodiment 5B is the composition of any one of Embodiments 1B-4B, wherein the polymer is a binder polymer.

[0111] Embodiment 6B is the composition of any one of Embodiments 1B-5B, wherein the polymer comprises one or more polyamides, polysulfones, polyethers, polyesters, polyamines, polyalcohols, polyurethanes, polycarbonates, polyaromatics, photopolymers, polyimides, polyacrylates, polyvinylidene fluorides, or combinations thereof.

[0112] Embodiment 7B is the composition of any one of Embodiments 1B-6B, wherein the electrospun nonwoven layer further comprises a conductive material.

[0113] Embodiment 8B is the composition of embodiment 7B, where the conductive material is carbon powder.

[0114] Embodiment 9B is the composition of any one of Embodiments 1B-7B, where the substrate is a current collector.

[0115] Embodiment 10B is the composition of embodiment 9B, wherein the substrate comprises a Cu foil, an Al foil, a Pt foil, a Ni foil, a woven substrate, a non-woven substrate, an artificial solid electrolyte interface, or a combination thereof.

[0116] Embodiment 11B is the composition of any one of Embodiments 1B-10B, where the substrate is made of silicon dioxide, aluminum dioxide, ceramic, or a combination thereof.

[0117] Embodiment 12B is the composition of any one of Embodiments 1B through 11B, wherein at least one chemical species is electroactive.

[0118] Embodiment 13B is the composition of embodiment 12B, wherein at least one compound species is LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, Li(Ni x Al y Co z)O2, or a combination thereof, where x+y+z=1. In some embodiments, the at least one compound species is Co3O4, Cu2O, Li4Ti5O 12 , SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO, and carbides thereof, LiAl alloy, LiSi alloy, LiBi alloy, LiCd alloy, AlMg alloy, LiMg alloy, LiSn alloy, LiSb alloy, FeSn alloy, SnSb alloy, SnCu alloy, LiGe alloy, LiPb alloy, oxides thereof, sulfides thereof, phosphides thereof, carbides thereof, and nitrides thereof; nitrides, oxides, and carbides of Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, and Sn; silicon; or combinations thereof.

[0119] Embodiment 14B is a composition according to any one of embodiments 1B-13B, wherein at least one of the compound species has catalytic activity.

[0120] Embodiment 15B is the composition of embodiment 14B, wherein at least one compound species comprises PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, TiO2, NiO, or combinations thereof. In some embodiments, at least one compound species comprises ZnO, ZnP, Ni2P, NiS, NiCo, NiCu, ZnO, NiO, Cu, AuPt, AuPd, TiO2, NiO, or combinations thereof.

[0121] Embodiment 16B is the composition of embodiment 1B, wherein the plurality of nanoparticles is a first plurality of nanoparticles, each nanoparticle comprising a first compound species, and the composition further comprises a second plurality of nanoparticles, each nanoparticle comprising a second compound species different from the first compound species.

[0122] [Embodiment C. Battery] Embodiment C1 is a battery comprising an electrode comprising the composition of any one of embodiments A or B.

[0123] Embodiment C2 is a battery that includes an electrode comprising a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one electroactive compound species, the plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm.

[0124] Embodiment C3 is the battery of embodiment C1 or C2, wherein the electrode is an electrospun nonwoven layer comprising a substrate and fibers deposited on the substrate by electrospinning, the fibers comprising a binder polymer and a plurality of nanoparticles dispersed on the binder polymer and throughout the fibers.

[0125] Embodiment C4 is the battery of any one of embodiments C1 to C3, wherein the plurality of nanoparticles have a particle size in the range of 0.02 μm to 0.4 μm.

[0126] Embodiment C5 is the battery of any one of embodiments C1-C4, wherein the at least one electroactive compound species is LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, and Li(Ni x Al y Co z )O2, where x+y+z=1. In some embodiments, the at least one compound species is Co3O4, Cu2O, Li4Ti5O 12, SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO, and carbides thereof, LiAl alloy, LiSi alloy, LiBi alloy, LiCd alloy, AlMg alloy, LiMg alloy, LiSn alloy, LiSb alloy, FeSn alloy, SnSb alloy, SnCu alloy, LiGe alloy, LiPb alloy, oxides thereof, sulfides thereof, phosphides thereof, carbides thereof, and nitrides thereof; nitrides, oxides, and carbides of Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, and Sn; silicon; or combinations thereof.

[0127] Embodiment C6 is the battery of one of embodiments C1-C5, wherein the fibers have an average diameter of less than 1.5 μm.

[0128] Embodiment C7 is the battery of any one of embodiments C1-C6, wherein the binder polymer comprises one or more polyamides, polysulfones, polyethers, polyesters, polyamines, polyalcohols, polyurethanes, polycarbonates, polyaromatics, photopolymers, polyimides, or combinations thereof.

[0129] Embodiment C8 is the battery of any one of embodiments C1-C7, wherein the substrate is a current collector.

[0130] Embodiment C9 is the battery of embodiment C8, in which the substrate is comprised of Cu foil, Al foil, Pt foil, Ni foil, a woven substrate, a non-woven substrate, an artificial solid electrolyte interface, or a combination thereof.

[0131] [Embodiment D. Method] Embodiment D1 is a method comprising electrospinning a solution onto a substrate, the solution comprising a binder polymer, a solvent, and a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one chemical species, the plurality of nanoparticles comprising a plurality of nanoparticles having a size range of 0.01 μm to 0.5 μm, and producing a nonwoven layer comprised of fibers comprising a binder polymer, a plurality of nanoparticles dispersed within the binder polymer and distributed throughout the fibers.

[0132] Embodiment D2 is the method of embodiment D1, wherein the fibers have an average diameter of less than 5 μm.

[0133] Embodiment D3 is the method of embodiment D1 or D2 wherein at least one chemical species is electroactive.

[0134] Embodiment D4 is the method of any one of embodiments D1-D3, wherein the at least one compound species is LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, and Li(Ni x Al y Co z )O2, where x+y+z=1. In some embodiments, the at least one compound species is Co3O4, Cu2O, Li4Ti5O 12 , SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO, and carbides thereof, LiAl alloy, LiSi alloy, LiBi alloy, LiCd alloy, AlMg alloy, LiMg alloy, LiSn alloy, LiSb alloy, FeSn alloy, SnSb alloy, SnCu alloy, LiGe alloy, LiPb alloy, oxides, sulfides, phosphides, carbides, and nitrides thereof; nitrides, oxides, and carbides of Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, and Sn; silicon; or combinations thereof.

[0135] Embodiment D5 is the method of any one of embodiments D1-D4, wherein at least one chemical species has catalytic activity.

[0136] Embodiment D6 is the method of embodiment D5 wherein the at least one compound species comprises PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, TiO2, NiO, or a combination thereof.

[0137] Embodiment D7 is a method comprising: forming a solution by dissolving at least one salt and a sacrificial polymer in a solvent, the solution comprising the sacrificial polymer, a first ionic species, a second ionic species, and the solvent; electrospinning the solution to form a sacrificial nonwoven material comprising fibers, the fibers comprising the sacrificial polymer and a first ionic species and a second ionic species dispersed on the polymer and distributed along the fibers; and decomposing at least a portion of the sacrificial nonwoven material, resulting in a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one chemical species, the at least one chemical species comprising a reaction product of at least the first ionic species and the second ionic species, the plurality of nanoparticles having a particle size range of 0.02 μm to 0.5 μm.

[0138] Embodiment D8 is the method of embodiment D7, further comprising spinning a mixture comprising a binder polymer and a plurality of nanoparticles onto a substrate, wherein electrospinning of the mixture results in a second nonwoven layer comprising second fibers comprising the binder polymer and nanoparticles from the plurality of nanoparticles dispersed within the binder polymer and distributed throughout the fibers.

[0139] Embodiment D9 is the method of embodiment D7 or D8, wherein at least one salt is LiNO3, LiH2PO4, Co(NO3)2, Ni(NO3)2, Fe(NO3)2, Mn(NO3)2, Al(NO3)3, Li2SO4, CoSO4, NiSO4, FeSO4, MnSO4, Al2(SO4)3, Fe(CH3COO)2, Al(OCH3)3, Al(CH3COO)3, or combinations thereof.

[0140] Embodiment D10 is the method of any one of embodiments D1-D9, wherein the at least one salt is selected from the group consisting of (NH4)AuCl4, NaAuBr, HAuCl4, KCl, KAuCl4, Na2PdCl4, K2PdBr4, PdCl6, K2PdCl6, (NH4)2PDCl4, K2PdCl4, Na2PtCl4, K2PtBr4, PtCl6, K2PtCl4, (NH4)2PtCl4, K2Pt(NO2)4, KAg(CN)2, KCu, Ni(NO3)2, Mg(NO3)2, NiCl2, PdCl2, Ni(Ac)2, NiBr2, NiI2, NiSO4, Pb(CH3COO)2, SeC l2, Se(CH3COO)2, SeBr4, ZnSO4, Zn(CH3COO)2, Zn(NO3)2, ZnCl2, FeCl2, FeSO4, Fe(NO3)2, RuCl3, Ru(NO3)3, RhCl3, Rh(NO3)3, IrCl4, Ir2(SO4)3, CuCl2, Cu(NO3)2 , CuSO4, Cu(CH3COO)2, SnCl4, Sn(CH3COO)2, SnSO4, Sn(NO3)4, AlCl3, Al2(SO4)3, Al(NO3)3, MgCl2, MgSO4, CoCl2, Co(CH3COO)2, CoSO4, Co(NO3)2, or combinations thereof.

[0141] Embodiment D11 is the method of any one of embodiments D1-D10, wherein the sacrificial polymer comprises polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, polyvinyl acetate, polyacrylonitrile, polyacrylate, polyamide, polysulfone, polyether, polyester, polyamine, polyalcohol, polyurethane, polycarbonate, polyaromatic, photopolymer, polyimide, or combinations thereof.

[0142] Embodiment D12 is the method of any one of Embodiments D1-D11, wherein at least one chemical species is electroactive.

[0143] Embodiment D13 is the method of embodiment D12, wherein the at least one compound species is LiCoO2, LiFePO4, LiMn2O4, LiNiO2, Li(Ni x Mn y Co z )O2, Li(Ni x Al y Co z )O2, or a combination thereof, where x+y+z=1. In some embodiments, the at least one compound species is Co3O4, Cu2O, Li4Ti5O 12 , SiO2, Fe2O3, Al3Ni, CuCo2O4, PdNiBi, TiO, Sn4P3, NiO, and carbides thereof, including LiAl alloys, LiSi alloys, LiBi alloys, LiCd alloys, AlMg alloys, LiMg alloys, LiSn alloys, LiSb alloys, FeSn alloys, SnSb alloys, SnCu alloys, LiGe alloys, LiPb alloys, oxides thereof, sulfides thereof, phosphides thereof, carbides thereof, and nitrides thereof; nitrides, oxides, and carbides of Li, Co, Pd, Pt, W, Mo, Zr, Fe, Al, Ni, Ti, and Sn; silicon; or combinations thereof.

[0144] Embodiment D14 is the method of any one of embodiments D1-D13, wherein at least one of the chemical species has catalytic activity.

[0145] Embodiment D15 is the method of embodiment D14, wherein the at least one compound species comprises PbSe, AuPt, AuPd, PtPd, PtRu, PtAg, PtCu, FeRu, FeCu, FeRh, CuCe, AuCu, PtIr, NiCu, NiSn, NiAl, PtAl2, PtMg, PtSn, PtCo, PdCo, ​​PdTi, PtRh, NiAu, RhAg, TiO2, NiO, or combinations thereof. In some embodiments, the at least one compound species comprises ZnO, ZnP, Ni2P, NiS, NiCo, NiCu, ZnO, NiO, Cu, AuPt, AuPd, TiO2, NiO, or combinations thereof.

[0146] Embodiment D16 is the method of any one of embodiments D1-D15, wherein the decomposing includes a heat treatment.

[0147] Embodiment D17 is the method of embodiment D16, wherein the heat treatment comprises pyrolysis at 500° C. to 1100° C. In some embodiments, the decomposition treatment 3 comprises pyrolysis at a temperature effective to decompose the sacrificial polymer to the desired extent, for example, 400° C. to 1100° C., 400° C. to 1000° C., 400° C. to 900° C., 400° C. to 800° C., 400° C. to 700° C., 400° C. to 600° C., 400° C. to 700° C., 500° C. to 1100° C., 500° C. to 1000° C., 500° C. to 900° C., 500° C. to 800° C., 500° C. to 700° C., or 500° C. to 600° C.

[0148] Embodiment D18 is the method of any one of embodiments D1-D17, wherein the solvent is selected from isopropanol, ethanol, methanol, dichloromethane, tetrahydrofuran, acetonitrile, acetone, N-methyl-2-pyrrolidone, water, benzyl alcohol, toluene, N,N'-dimethylformamide, acetic acid, formic acid, or a combination thereof.

[0149] Embodiment D19 is the method of embodiment D18 wherein the first solvent and the second solvent are each independently selected from isopropanol, ethanol, methanol, dichloromethane, tetrahydrofuran, acetonitrile, acetone, N-methyl-2-pyrrolidone, water, benzyl alcohol, toluene, N,N'-dimethylformamide, acetic acid, formic acid, or combinations thereof.

[0150] Embodiment D20 is the method of any one of embodiments D1-D19, wherein the binder polymer is selected from polyamides, polysulfones, polyethers, polyesters, polyamines, polyalcohols, polyurethanes, polycarbonates, polyaromatics, photopolymers, polyimides, polyvinyl acetates, polyacrylonitriles, polyacrylates, polyvinylidene fluorides, or combinations thereof.

[0151] Embodiment D21 is the method of any one of embodiments D1-D20, wherein the plurality of nanoparticles have a particle size in the range of 0.02 μm to 0.4 μm.

[0152] Embodiment D22 is the method of embodiment D21, wherein the first fibers and the second fibers each independently have an average diameter of 5 μm or less, 4 μm or less, 3 μm or less, 2 μm or less, 1.5 μm or less, 1.2 μm or less, 1.0 μm or less, 0.8 μm or less, 0.6 μm or less, 0.4 μm or less, or 0.2 μm or less. In some embodiments, the first fibers and the second fibers each independently have an average diameter of at least 0.1 μm, at least 0.2 μm, at least 0.4 μm, at least 0.5 μm, at least 0.6 μm, at least 0.8 μm, at least 1.0 μm, or at least 1.2 μm. In some embodiments, the first fibers and the second fibers each independently have a diameter of 0.1 μm to 5 μm, 0.1 μm to 4 μm, 0.1 μm to 3 μm, 0.1 μm to 2 μm, 0.5 μm to 5 μm, 0.5 μm to 4 μm, 0.5 μm to 3 μm, 0.5 μm to 2 μm, 0.8 μm to 5 μm, 0.8 μm to 4 μm, 0. having an average diameter of 8 μm to 3 μm, 0.8 μm to 2 μm, 1 μm to 5 μm, 1 μm to 4 μm, 1 μm to 3 μm, 0.1 μm to 1.5 μm, 0.2 μm to 1.5 μm, 0.4 μm to 1.5 μm, 0.6 μm to 1.5 μm, 0.8 μm to 1.5 μm, 1.0 μm to 1.5 μm, or 1.2 μm to 1.5 μm.

[0153] [Embodiment E. Composition] Embodiment E1 is a composition prepared by the method of any one of Embodiments D.

[0154] <Example> Exemplary methods for preparing nanoparticles and possible applications of such nanoparticles are illustrated by the following examples, it being understood that the specific examples, materials, amounts, and procedures are to be broadly interpreted in accordance with the scope and spirit of the present disclosure.

[0155] <Example 1> Example 1 describes a process for producing a plurality of nanoparticles, each nanoparticle containing an electroactive compound species having cathodic electroactivity. Seven solutions were prepared for electrospinning and subsequent heat treatment. [Table 1]

[0156] <Solution 1> A solution of 5% (w / v) polyvinylpyrrolidone (PVP) and 5% (w / v) total lithium and cobalt nitrates (Li:Co molar ratio 1:1) in a mixed solvent of isopropyl alcohol (IPA) and N,N-dimethylformamide (DMF) 1:1 (v / v) was used as the electrospinning precursor for lithium cobalt oxide (LiCoO2, LCO) fibers. The precursor solution was prepared by dissolving 0.9577 g of lithium nitrate (LiNO3) and 4.074 g of cobalt(II) nitrate hexahydrate (Co(NO3)2·6H2O) in 100 mL of the mixed solvent (50 mL of IPA and 50 mL of DMF). 5.0 g of PVP was slowly added to the solution under magnetic stirring to avoid clumping. The precursor solution was stirred overnight at room temperature to completely dissolve the PVP and metal salts.

[0157] <Solution 2> A solution of 5% (w / v) polyvinylpyrrolidone (PVP) and 5% (w / v) total of lithium nitrate and nickel nitrate (Li:Ni molar ratio 1:1) in a 1:1 (v / v) mixed solvent of IPA and DMF was used as the electrospinning precursor for lithium cobalt oxide (LiNiO2, LNO) fibers. The precursor solution was prepared by dissolving 0.9580 g of lithium nitrate (LiNO3) and 4.050 g of nickel(II) nitrate hexahydrate (Ni(NO3)2·6H2O) in 100 mL of the mixed solvent (50 mL IPA and 50 mL DMF). 5.0 g of PVP was slowly added to the solution under magnetic stirring to avoid clumping. The precursor solution was stirred at room temperature overnight to completely dissolve the PVP and metal salts.

[0158] <Solution 3> A solution of 5% (w / v) nylon SVP 651 and 5% (w / v) total lithium and cobalt nitrates (Li:Co molar ratio 1:1) in ethanol (EtOH, 190 proof) was used as electrospinning precursor for lithium cobalt oxide (LiCoO2, LCO) fibers. The precursor solution was prepared by dissolving 0.9577 g of lithium nitrate (LiNO3) and 4.074 g of cobalt(II) nitrate hexahydrate (Co(NO3)2·6H2O) in 100 mL of EtOH. 5.0 g of SVP 651 was added slowly to the solution with magnetic stirring to prevent agglomeration. The precursor solution was stirred overnight while heating to 60 °C under reflux conditions to completely dissolve all solids.

[0159] <Solution 4> A solution of 5% (w / v) nylon SVP 651 and 5% (w / v) total lithium and nickel nitrates (Li:Ni molar ratio 1:1) in ethanol (EtOH, 190 proof) was used as electrospinning precursor for lithium cobalt oxide (LiNiO2, LNO) fibers. The precursor solution was prepared by dissolving 0.9580 g of lithium nitrate (LiNO3) and 4.050 g of nickel(II) nitrate hexahydrate (Ni(NO3)2·6H2O) in 100 mL of EtOH. 5.0 g of SVP 651 was added slowly to the solution with magnetic stirring to prevent agglomeration. The precursor solution was stirred overnight while heating to 60 °C under reflux conditions to completely dissolve all solids.

[0160] <Solution 5> A solution of 7.5% (w / v) nylon SVP 651 and 10% (w / v) total lithium, nickel, manganese and cobalt nitrates (Li:Ni:Mn:Co molar ratio 1:0.8:0.1:0.1) in ethanol (EtOH, 190 proof) was used as the electrospinning precursor for lithium nickel manganese cobalt oxide (NMC 811) fibers. The precursor solution was prepared by dissolving 1.941 g lithium nitrate (LiNO3), 6.540 g nickel(II) nitrate hexahydrate (Ni(NO3))2·6H2O), 0.7054 g manganese(II) nitrate tetrahydrate (Mn(NO3))2·4H2O) and 0.8103 g cobalt(II) nitrate hexahydrate (Co(NO3)2·6H2O) in 100 mL EtOH. 7.5 g of SVP 651 was slowly added to the solution with magnetic stirring to prevent agglomeration. The precursor solution was stirred overnight under reflux conditions while being heated to 60° C. until all solids were completely dissolved.

[0161] <Solution 6> A solution of 7.5% (w / v) nylon SVP 651 and 10% (w / v) total lithium, nickel, cobalt, and aluminum nitrates (Li:Ni:Co:Al molar ratio 1:0.8:0.15:0.05) in ethanol (EtOH, 190 proof) was used as the electrospinning precursor for lithium nickel cobalt aluminum oxide (NCA) fibers. The precursor solution was prepared by dissolving 1.8944 g lithium nitrate (LiNO3), 6.3909 g nickel(II) nitrate hexahydrate (Ni(NO3)2·6H2O), 1.201 g cobalt(II) nitrate hexahydrate (Co(NO3)2·6H2O), and 0.5152 g aluminum(III) nitrate nonhydrate (Al(NO3)3·9H2O) in 100 mL EtOH. 7.5 g of SVP 651 was slowly added to the solution with magnetic stirring to prevent agglomeration. The precursor solution was stirred overnight under reflux conditions while being heated to 60° C. until all solids were completely dissolved.

[0162] <Solution 7> A solution of 7.5% (w / v) nylon SVP 651 and 10% (w / v) total lithium, nickel, manganese, and cobalt nitrates (Li:Ni:Mn:Co molar ratio 1:0.6:0.2:0.2) in ethanol (EtOH, 190 proof) was used as the electrospinning precursor for lithium nickel manganese cobalt oxide (NMC 622) fibers. The precursor solution was prepared by dissolving 1.941 g lithium nitrate (LiNO3), 4.9050 g nickel(II) nitrate hexahydrate (Ni(NO3))2·6H2O), 1.4108 g manganese(II) nitrate tetrahydrate (Mn(NO3))2·4H2O), and 1.6206 g cobalt(II) nitrate hexahydrate (Co(NO3)2·6H2O) in 100 mL of EtOH. 7.5 g of SVP 651 was slowly added to the solution with magnetic stirring to prevent agglomeration. The precursor solution was stirred overnight under reflux conditions while being heated to 60° C. to completely dissolve all solids.

[0163] <Electrospinning> Samples of solutions 1-6 were prepared by filling a pendant dropping apparatus, i.e. a syringe, with the polymer solution. A high voltage is applied to a needle attached to the syringe, and the polymer solution is pumped at a given pumping speed. As a droplet of the polymer solution leaves the needle, it is influenced by an electrostatic field (field) to form a Taylor cone. At a sufficiently high voltage, a jet is emitted from the Taylor cone, which elongates to form fine fibers, which are deposited onto a media attached to a rotating mandrel that acts as a collector.

[0164] The fibers were formed by electrospinning onto a support layer wound around a cylinder (10.16 cm diameter, rotating at 300 rpm) at a voltage of 24 kV, a distance of 10.16 cm from the syringe or syringes delivering the polymer solution, and a pump rate of 0.02 mL / min. After electrospinning, the formed fine fibers were stored in a desiccator before subsequent heat treatment at 550 °C for 1 h.

[0165] Six nonwoven fiber layers from samples prepared from solutions 1-6 were fabricated with a basis weight of 70 g / m by electrospinning solutions 1-6 four times separately. 2 , and were separately deposited onto a 0.2 mm thick spunbond nylon scrim (Media Grade 23200) with 28% solids. The solutions were pumped at the same pump rate (0.02 mL / min) for the same time (5 min).

[0166] FIG. 5 shows a scanning electron microscope image of fibers formed from electrospinning solution 3 of Example 1.

[0167] FIG. 6 shows a scanning electron microscope image of fibers formed from electrospinning solution 5 of Example 1.

[0168] FIG. 7 shows a scanning electron microscope image of fibers formed from electrospinning solution 6 of Example 1.

[0169] <Heat treatment> All samples underwent post-electrospinning treatment to convert the as-spun nonwovens into cathode active materials. After electrospinning, the formed fibers were peeled off from the substrate and placed in a ceramic boat lined with aluminum foil. Before loading the samples into a quartz tube furnace, the furnace was preheated to 100 °C and maintained at the elevated temperature for 20 min using dry compressed air as a purge gas to remove moisture from the furnace walls. The electrospun fibers were then placed into the tube furnace and heat treated at 550 °C for 1 h using the same dry compressed air. A heating rate of 20 °C / min was used for the heating ramp.

[0170] Figures 8 and 9 are transmission electron microscopy images of LiCoO2 nanoparticles formed after decomposition treatment of the sacrificial nonwoven material made from Solution 3. Figure 9 shows a uniform thin amorphous carbon coating formed in situ around the individual highly crystalline nanoparticles.

[0171] The heat-treated samples were subjected to crystallinity measurement by X-ray scattering spectroscopy using a diffractometer in reflection mode. The D8 DISCOVER 2D X-ray microdiffractometer (available from Bruker Corporation, Billerica, MA) is equipped with a 2D VANTEC detector, a video camera / laser alignment system, and a Co Kα X-ray radiation point source (1 = 1.79 Å) aligned with a graphite monochromator. It is also equipped with point collimators of various sizes and x, y, z sample stages. The samples were fixed on the Si wafer using as-received paste without breaking the crystals into fine powder. The samples were aligned separately in the x, y, and z directions. An 800 μm collimator was used and the sample-to-detector distance was kept at 20 cm. 20 / 10, 40 / 20, 60 / 30, 20 frames each were scanned for 600 seconds using JPEG2024542801000003.jpg1064. Area detector images were converted to one-dimensional intensity vs. 2θ data sets using an averaging integration algorithm. Patterns were converted to polar coordinates using GADDS.

[0172] Figure 10 shows the X-ray spectrum of LiCoO2 nanoparticles formed after decomposition treatment of the sacrificial nonwoven material prepared from Solution 3. The nanoparticles show high crystallinity and no amorphous content.

[0173] [Example 2A] Example 2A describes a manufacturing process for a cathode assembly. Nanoparticles produced according to Example 1 are isolated. The isolated nanoparticles and a binder polymer are electrospun to form a nonwoven layer on a current collector substrate.

[0174] After the heat treatment step of Example 1, the nanoparticles can be isolated from the sample using conventional techniques such as filtration and sieving. Additionally, nanoparticles of a desired size can be isolated using additional filter techniques.

[0175] The isolated nanoparticles, conductor material, and binder polymer can be dissolved in a solvent that produces a homogenous mixture. The solvent can be selected to suppress dissociation of the nanoparticles into their constituent ionic species. This solution can be electrospun according to the conditions provided in Example 1, except that the media attached to the rotating mandrel is a material suitable as a current collector. If the media attached to the rotating mandrel is not a suitable material as a current collector, the nonwoven layer can be removed from the mandrel media and attached to a material suitable as a current collector after the electrospinning process.

[0176] The nonwoven layer may be subjected to post-electrospinning treatments, such as placing the nonwoven layer in a desiccator or adhering the nonwoven layer to a current collector by known mechanical and chemical processes.

[0177] [Example 2B] Samples were prepared from three mixtures containing polymer, carbon black particles, and solvent. Carbon black particles were used instead of lithium cobalt oxide (LiCoO2, LCO) particles.

[0178] <Mixture 1> PVdF (10% w / v) and Timcal Super C65 conductive carbon black (30% w / w) were mixed in a mixture of DMF and acetone (6:4 v / v). This mixture was mixed at 2000 rpm for 10 min using a FlackTek 330-100 speed mixer and then used as the electrospinning solution for testing.

[0179] <Mixture 2> 10% (w / v) PVdF and 50% (w / w) Timcal Super C65 conductive carbon black were mixed in a 6:4 (v / v) mixture of DMF and acetone. This mixture was mixed at 2000 rpm for 20 min using a FlackTek 330-100 speed mixer and then used as the electrospinning solution for testing.

[0180] <Mixture 3> 15% (w / v) PVdF and 3.8% (w / w) Timcal Super C65 conductive carbon black were mixed in a 6:4 (v / v) mixture of DMF and acetone. This mixture was mixed at 2000 rpm for 20 minutes using a FlackTek 330-100 speed mixer and then used as the test electrospinning solution. This percentage of C65 solids is consistent with a number of conductive materials currently used in commercial applications, typically 3% (w / w).

[0181] <Electrospinning> Samples of Mixtures 1-3 were prepared using a pendant drop apparatus as described above for Example 1.

[0182] Fibers were formed by electrospinning onto a cylindrical support layer (Reynolds Wrap Aluminum Foil Wrap) (diameter 10.16 cm, rotating at 300 rpm) at various voltages and pump speeds with a set run time of 5 minutes.

[0183] Two samples were prepared and run using Mixture 1. Both samples were run with a syringe-to-collector distance of 8 cm and a flow rate of 0.75 mL / hr. Sample 1A was collected at a voltage of 20 kV and Sample 1B at a voltage of 15 kV. Both samples were then cut and glued onto SEM stubs, sputter coated using silver for better visibility, and analyzed using a SEM (JEOL JSM-5900LV) and properties such as fiber diameter were recorded using the program's scalar measurement tool. SEM images are shown in Figure 11A (Sample 1A) and Figure 11B (Sample 1B).

[0184] Sample 2 was run using mixture 2 with a syringe-to-collector distance of 10 cm, voltage of 8 kV, and pump speed of 1 mL / hr. The sample was then cut and glued to an SEM stub, sputter coated with silver for better visibility, and analyzed using a SEM (JEOL JSM-5900LV). The SEM image is shown in Figure 12.

[0185] Four samples (3A, 3B, 3C, 3D) were run using mixture 3. Each sample was prepared with a syringe-to-collector distance of 10 cm. The first two (3A and 3B) were both run at a rate of 7.5 mL / h, one sample (3A) at a voltage of 20 kV, and the other (3B) at a voltage of 30 kV. The last two (3C and 3D) were both run at a voltage of 25 kV, with pump rates of 10 mL / h (3C) and 5 mL / h (3D). The samples were then cut and glued onto SEM stubs, sputter-coated with silver for better visibility, and analyzed using a SEM (JEOL JSM-5900LV). The SEM images are shown in Figure 13A (sample 3A), 13B (sample 3B), 13C (sample 3C), and 13D (sample 3D).

[0186] [Example 3] The positive electrode assembly of Example 2 can be used in a lithium ion battery.

[0187] The effectiveness of the cathode assembly of Example 2 in a battery setting can be tested by employing the cathode assembly in a lithium-ion coin cell. The lithium-ion coin cell containing the cathode assembly of Example 2 can be used to evaluate various properties of the cathode assembly, including C-rate, areal and volumetric capacity at high and low charge and discharge rates, capacity retention, energy density, and cathode stability during use.

[0188] [Example 4] The catalytic assemblies can be fabricated using the processes described in Examples 1 and 2, but with some differences. First, instead of nanoparticles containing cathodically active compounds, the nanoparticles of the catalytic assemblies contain catalytically active compounds. Therefore, the salt used to make the electrospinning solution is a salt that can dissolve into ionic species that can react to form catalytically active compounds. Second, instead of a current collecting substrate, the substrate is made of a material that helps or does not hinder the catalytic reaction. Third, the catalytic assemblies may not require conductive members.

[0189] [Example 5] A cathode assembly using the active material of Example 1 can be fabricated by conventional slurry casting techniques and used in lithium ion batteries.

[0190] The effectiveness of the cathode assembly in a battery environment can be tested by employing the cathode assembly in a lithium-ion coin cell. The lithium-ion coin cell containing the cathode assembly can be used to evaluate various properties of the cathode assembly, including C-rate, areal and volumetric capacity at high and low charge and discharge rates, capacity retention, energy density, and cathode stability during use.

[0191] <Mixture 4> a) LiNi prepared as described from solution 7 in Example 1 0.6 Mn 0.2 Co 0.2 A mixture of O2 (NMC 622) nanoparticles, b) 8 wt% polyvinylidene fluoride (PVdF, molecular weight = 630,000 g / mol) in N-methyl-2-pyrrolidone, and c) Timcal Super C65 conductive carbon black was mixed in a mass ratio of 94:3:3 using a FlackTek 330-100 speed mixer at 2000 rpm for 10 min.

[0192] <Cathode assembly by slurry casting> Mixture 4 was applied as a wet film (150-180 μm thick) onto an aluminum foil current collector (14-15 μm thick) by slurry casting using an AFA-III Automatic Thick Film Coater (available from MTI Corporation). The film was then transferred to a vacuum oven (Fisher Scientific Isotemp Vacuum Oven Model 282A) heated to 110 °C at 15 mm Hg and dried for at least 1 hour. The dried cathode assembly was then calendered at ambient temperature to a final thickness of 60 μm using a benchtop hot rolling press such as MSK-HRP-01 (MTI Corporation). The total mass loading on a dry basis was approximately 10 mg / cm. 2It is.

[0193] An SEM image of a cathode assembly using NMC622 from Example 1 is shown in FIG. 14A.

[0194] <Coin Cell Assembly and Testing> The cathode assembly was transferred to an argon glove box and used as the positive electrode in a CR2032 coin cell in a half-cell configuration against lithium metal foil separated by a Celgard separator and using 1M LiPF6 in a 3 / 7 ethyl carbonate / ethyl methyl carbonate solvent mixture as the electrolyte: a) initial charge at 0.1C rate, b) three charge-discharge cycles at 0.1C rate, c) charge-discharge cycles at 1C rate until the total discharge capacity dropped to at least 10% of the initial discharge capacity (measured from cycle 1).

[0195] A plot of the measured discharge capacity with increasing number of charge / discharge cycles is shown in Figure 14B, and a plot of the measured coulombic efficiency with increasing number of charge / discharge cycles is shown in Figure 14C.

[0196] All references and publications cited herein are expressly incorporated by reference in their entirety into this disclosure, except to the extent that they may directly contradict this disclosure. Although specific embodiments have been illustrated and described herein, those skilled in the art will understand that various alternative and / or equivalent embodiments may be substituted for the specific embodiments illustrated and described without departing from the scope of the present disclosure. The present disclosure is not intended to be unduly limited by the exemplary embodiments and examples described herein, which are presented solely as examples with the intent that the scope of the present disclosure be limited only by the claims set forth herein.

[0197] All headings are for the convenience of the reader and should not be used to limit the meaning of the text that follows the heading, unless specifically stated.

Claims

1. 1. A composition comprising an electrospun nonwoven material comprising fibers having an average diameter of less than 5 μm, The fibers are a sacrificial polymer present at 40% to 60% by weight of the total weight of the electrospun nonwoven layer; and a first ionic species and a second ionic species dispersed on the sacrificial polymer and distributed along the fibers; Including, the first ionic species and the second ionic species are ionic species of at least one salt, and the at least one salt is present at 60% by weight or less of the total salt; A composition wherein the weight percent of said total salts relative to the weight percent of said sacrificial polymer is greater than or equal to 1 part by weight percent of said total salts relative to 6 parts by weight percent of said sacrificial polymer.

2. 10. The composition of claim 1, wherein the at least one salt is NiCl. ２ , Ni(CH ３ COO) ２ , ZnSO ４ , Zn(CH ３ COO) ２ , KCl, KAuCl ４ , CoCl ２ , Co(CH ３ COO) ２ , CuCl ２ , Cu(NO ３ ) ２ , PdCl ６ , K. ２ PdCl ６ , Na ２ PtCl ４ , K. ２ PtBr ４ , Ni(NO ３ ) ２ , Co(NO ３ ) ２ , Mn(NO ３ ) ２ , Al(NO ３ ) ３ , Fe(NO ３ ) ２ , LiNO ３ , LiH ２ P.O. ４ , Fe(CH ３ COO) ２ , NiSO ４ , CoSO ４ , Li ２ SO ４ , MnSO ４ , FeSO ４ , Al ２ (SO ４ ) ３ , Al(OCH ３ ) ３ , Al(CH ３ COO) ３ or a combination thereof.

3. 10. The composition of claim 1, wherein the sacrificial polymer is polyvinylpyrrolidone, polyethylene glycol, nylon, polyurethane, polyvinyl alcohol, polyvinyl acetate, polyacrylonitrile, polyacrylate, or a combination thereof.

4. a substrate, and a first fiber layer comprising fibers deposited on the substrate by electrospinning; 1. A composition comprising the electrospun nonwoven layer, wherein the fibers comprise: a first polymer, and a first plurality of nanoparticles dispersed on the polymer and distributed throughout the fibers, the first plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm, each nanoparticle comprising a plurality of at least one chemical species.

5. The composition of claim 4 further comprising: a second fiber layer including second fibers deposited on the first fibers by the electrospinning, the second fibers comprising: a second polymer, and a second plurality of nanoparticles dispersed on the second polymer and distributed throughout the fibers, the second plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm, each nanoparticle comprising a plurality of at least one compound species; Including, The composition, wherein the first fibrous layer has a density at least 1.1 times the density of the second fibrous layer.

6. A battery, an electrode comprising an electrospun nonwoven layer comprising a plurality of nanoparticles, each nanoparticle comprising a plurality of at least one electroactive compound species, said plurality of nanoparticles having a particle size range of 0.01 μm to 0.5 μm; The electrospun nonwoven layer comprises a substrate and fibers deposited on the substrate by electrospinning, the fibers comprising: a binder polymer; the plurality of nanoparticles dispersed on the binder polymer and distributed throughout the fibers.

7. Dissolving at least one salt and a sacrificial polymer in a solvent to form a solution, said solution comprising: The sacrificial polymer a first ionic species; a second ionic species, and The solvent forming the solution, electrospinning the solution to form a sacrificial nonwoven layer comprising fibers, the fibers comprising: the sacrificial polymer, and the electrospinning step including the first ionic species and the second ionic species dispersed on the polymer and distributed along the fiber; A method comprising:

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