Time-of-flight Secondary Ion Mass Spectrometry Research Articles

Mixed-cation, mixed-halide perovskite ToF-SIMS spectra

We report positive and negative ion time-of-flight secondary ion mass spectrometry (ToF-SIMS) spectra of metal-halide perovskite (MHP) films used for photovoltaic applications. This ToF-SIMS spectral library is of importance because it identifies the major peaks in most MHP films from organic [formamidinium (FA+)] and inorganic (Cs+) cations and anions (I− and Br−).

Precise determination of oxygen content in SmBa2Cu3O7-δ thin film samples using x-ray diffraction

Abstract The superconducting properties of SmBa2Cu3O7-δ (SmBCO) thin films are predominantly influenced by the oxygen deficiency δ. Yet, the established methods to determine δ such as iodometric titration or thermogravimetry cannot be applied to thin films due to their very small volume.
Therefore, an alternative way to determine δ for SmBCO thin film samples using X-ray diffraction (XRD) is presented. Main point of this analysis is the structural relationship between the a, b and c lattice parameters and δ. A linear relationship between c and δ is found in SmBCO powder samples for both the orthorhombic and tetragonal phases.
Furthermore, an attempt is made to quantify the chemical composition using Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). This attempt was inconclusive because of drastically changing ion yields due to δ influencing the valence state of the analyzed ions.
The found crystal structural relationship gathered from the powder samples is applied to thin film samples. Thereby, it becomes clear that thermal strain is affecting the crystal structure of the thin films. A simple correction model is used to correct for thermal strain and a good match between powder, literature and thin film data is achieved and thus a non-destructive way for the determination of δ using XRD.


Recyclable organic radical electrodes for metal-free batteries.

Organic batteries are one of the possible routes for transitioning to sustainable energy storage solutions. However, the recycling of organic batteries, which is a key step toward achieving circularity, is not easily achieved. This work shows the direct recycling of poly(2,2,6,6-tetramethylpiperidinyloxy-4-yl) (PTMA) and poly(2,2,6,6-tetramethylpiperidinyloxy-4-yl acrylamide) (PTAm) based composite electrodes. After charge-discharge cycling, the electrodes are deconstructed using a solubilizing-solvent and then reconstructed using a casting-solvent. The electrochemical properties of the original and recycled electrodes are compared using cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) cycling, from which it is discovered using time-of-flight secondary ion mass spectrometry (ToF-SIMS) that recycling can be challenged by the formation of a solid-electrolyte interphase (SEI). In turn, an additive is proposed to modify the SEI layer and improve the properties after recycling. Last, an anionic rocking chair battery consisting of PTAm electrodes as both positive and negative electrodes is demonstrated, in which the electrodes are recycled to form new battery. This work gives demonstrates the recycling of composite electrodes for organic batteries and provides insights into the challenges and possible solutions for recycling the next-generation electrochemical energy storage devices.

Preparation and formation mechanism of high-toughness organic polymers modified geopolymers

In recent years, geopolymers have shown potential to replace ordinary cement materials due to their simple preparation, low cost, and excellent performance. Adding organics to geopolymers can enhance toughness and broaden their application potential as building materials. However, the effect of common molding processes to enhance the toughness of organic polymers modified geopolymers remains very limited. In this study, high-toughness organic polymers modified geopolymers were prepared using vacuum-vibration-compaction (VVC) molding. The incorporation of 3-methacryloy loxypropyl trimethoxysilane (KH570) and sodium polyacrylate (PAAS), (KH-PAAS), was evaluated on the toughness system of the slag-based geopolymers. The micromechanical properties of the different hydrated phases were analyzed using a nano-scratch test (NST) and atomic force microscopy (AFM). The high fracture toughness (1.6–2.6 MPa*m0.5) and low elastic modulus (20–30 GPa) of the hydrated new phase C-(A)-S-H/Polymer gels were proposed. KH-PAAS modified geopolymers produced 57–59 % C-(A)-S-H/Polymer gels in which C-(A)-S-H/Polymer gels, C-(A)-S-H gels, and KH-PAAS were planarly cross-distributed to form a 3D network structure. The toughness of KH-PAAS modified geopolymers is related to the amount of C-(A)-S-H/Polymer gels generation and distribution form. Finally, the formation mechanism of the C-(A)-S-H/Polymer gels was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to quantify the ratio of different chemical reactions. The specific ratio was C-(A)-S-H-KH: C-(A)-S-H-PAAS: Ca-PAAS: KH–C-(A)-S-H-PAAS = 2.42 : 6.78: 47.58 : 1. This study provides ideas for subsequent investigation of the toughening mechanism of organic polymers modified geopolymers.

Quantitative analysis of molecular interactions in κ-carrageenan-Isovanillin biocomposite for biodegradable packaging and pharmaceutical applications using NMR, TOF-SIMS, and XPS approach

This study explores the molecular interactions and structural changes in κ-carrageenan crosslinked with isovanillin to create a biocomposite material suitable for hard capsule and bio-degradable packaging applications. Proton Nuclear Magnetic Resonance (1H NMR) spectroscopy revealed chemical changes in the conjugate molecule, indicating improved electronegativity due to intermolecular hydrogen bonding between κ-carrageenan and isovanillin. Time-of-flight Secondary Ion Mass Spectrometry (ToF-SIMS) analysis revealed enhanced ion intensity due to intermolecular interactions, particularly between sulphate and hydrogen ions. X-ray Photoelectron Spectroscopy (XPS) study demonstrated that κ-carrageenan and isovanillin form stronger hydrogen bonds, with a shift in binding energy indicating higher electronegativity. These findings shed light on the molecular mechanisms that underpin the formation of the biocomposite material, as well as its potential for use in hard capsule and biodegradable packaging materials, addressing the need for sustainable alternatives in the pharmaceutical and packaging industries while also contributing to environmental conservation.

Investigation on nanoindentation and TOF-SIMS applications in the hydrogen and oxygen absorption behavior of Zr-Sn-Nb alloys

This paper focuses on nanoindentation and TOF-SIMS (time-of-flight secondary ion mass spectrometry) small-scale test methods in the study of hydrogen absorption and oxygenation behavior analysis of Zr-Sn-Nb oxidized at 650°C -1200 °C. The CSM (Continuous Stiffness Method) test demonstrates the hardness fluctuations caused by element proliferation in post-high temperature oxidation microstructures. The deformation resistance ability of typical microstructures is as follows: β-Zr layer > α-Zr(O) layer > ZrO2 layer. In addition, hydrogen-induced softening occurred in steam-containing hydrogen conditions (HIT=2～3Gpa), compared to steam (HIT=5～16Gpa). The 1200℃ load-displacement curve demonstrates that the pop-in (or pop-out) effect exists in the Zr-Sn-Nb alloy, related to the influence of hydrogen charge, essentially to dislocation nucleation, winding, and movement. TOF-SIMS provides an effective method for small molecular chemical elements, such as H and O, while ZrO, ZrO2, ZrO2H, ZrO3H, OH, and O2 ions also be found. Based on these results, this study also hypothesizes the OH- dominated oxidation reaction equation.

Enhancement imaging of developed latent blood fingerprints using TOF-SIMS

As one of the most common types of evidence in violent cases, blood fingerprints play an important role in identifying suspects. Typically, Latent blood fingerprints from a crime scene require the application of chemical development reagents followed by photographing to visualize the ridge detail. However, conventional development techniques are not effective in the visualization of poor latent blood fingerprints due to the formation conditions. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a surface analysis technique that combines high mass resolution and high spatial resolution to recover through mass spectrometry imaging (MSI) to reveal fingerprints that are invisible to the naked eye, especially conventional visualization methods. In this study, an enhancement method for latent blood fingerprints was established by analyzing blood fingerprints that showed poor visibility using conventional methods (acid yellow, amido black 10B, tetramethylbenzidine) on plastic sheets, aluminum foil, various papers, and other objects. Additionally, blood samples were diluted with distilled water at concentration gradients of 1:5, 1:10, 1:20, and 1:100 to test the method's sensitivity. Latent fingerprints of blood that aged 14, 30, and 54 days were also examined. Results showed that this method not only enhances the development of fingerprints under challenging conditions but also allows for the recovery of incomplete fingerprints and the separation of overlapping fingerprints. Compared to conventional methods, this approach significantly improves the development effect of latent blood fingerprints while maintaining universality, reliability and practicality.

Application of operando ORP-EIS for the in-situ monitoring of acid anion incorporation during anodizing

Operando odd random phase electrochemical impedance spectroscopy (ORP-EIS) is applied to monitor the anodizing process of AA2024 in acidic media. The impedance data reveals the presence of inductive behavior during the process. We correlate this inductive behavior to the acid anion incorporation during anodizing using the surface charge approach. Moreover, the impact of anodizing parameters—including anodizing DC potential, electrolyte type and concentration—is studied on the inductive behavior, and consequently on the acid anion adsorption and incorporation. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is employed to support the operando ORP-EIS results. We conclude that operando ORP-EIS during anodizing can predict acid anion incorporation into the oxide layer.

Exploring chitosan-plant extract bilayer coatings: Advancements in active food packaging via polypropylene modification

UV-ozone activated polypropylene (PP) food films were subjected to a novel bilayer coating process involving primary or quaternary chitosan (CH/QCH) as the first layer and natural extracts from juniper needles (Juniperus oxycedrus; JUN) or blackberry leaves (Rubus fruticosus; BBL) as the second layer. This innovative approach aims to redefine active packaging (AP) development. Through a detailed analysis by surface characterization and bioactivity assessments (i.e., antioxidant and antimicrobial functionalities), we evaluated different coating combinations. Furthermore, we investigated the stability and barrier characteristics inherent in these coatings. The confirmed deposition, coupled with a comprehensive characterization of their composition and morphology, underscored the efficacy of the coatings. Our investigation included wettability assessment via contact angle (CA) measurements, X-ray photoelectron spectroscopy (XPS), and attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), which revealed substantial enhancements in surface concentrations of elements and functional groups of CH, QCH, JUN, and BBL. Scanning electron microscopy (SEM) unveiled the coatings' heterogeneity, while time-of-flight secondary ion mass spectrometry (ToF-SIMS) and CA profiling showed moderately compact bilayers on PP, providing active species on the hydrophilic surface, respectively. The coatings significantly reduced the oxygen permeability. Additionally, single-layer depositions of CH and QCH remained below the overall migration limit (OML). Remarkably, the coatings exhibited robust antioxidative properties due to plant extracts and exceptional antimicrobial activity against S. aureus, attributed to QCH. These findings underscore the pivotal role of film surface properties in governing bioactive characteristics and offer a promising pathway for enhancing food packaging functionality.

Synergistic inhibition of Mikania micrantha extract with iodide ion on the corrosion of cold rolled steel in trichloroacetic acid medium

The corrosion inhibition behavior of Mikania micrantha extract (MME) and iodide ion in a synergistic system consisting of 0.10 M trichloroacetic acid (Cl3CCOOH, TCA) on cold rolled steel (CRS) materials and its mechanism was fully investigated by weightlessness, electrochemical, and surface analysis measurements. The results show that MME/I− performs higher inhibition than either MME or I− with a peak inhibition efficiency of 96.3 %. The adsorption of MME, I− and MME/I− on CRS follow with Langmuir isotherm. MME/I− retards both anodic and cathodic reactions. With the MME/I− complex inhibitor, the capacitance arc radius reaches a maximum. The results of scanning electron microscopy (SEM), atomic force microscopy (AFM), and confocal laser scanning microscopy (CLSM) showed that there were obvious adsorbent films on the surface of the suppressed CRS. Compositional analysis of surface adsorbates on CRS by X-ray photoelectron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (TOF-SIMS) revealed that the main components of the adsorption film on the surface of CRS contained a large number of polar compounds, notably the formation of chemical bonds by iron atoms.

Exploring the Performance of Linear and Nonlinear Models of Time-of-Flight Secondary Ion Mass Spectrometry Spectra.

Multivariate statistical tools and machine learning (ML) techniques can deconvolute hyperspectral data and control the disparity between the number of samples and features in materials science. Nevertheless, the importance of generating sufficient high-quality sample replicates in training data cannot be overlooked, as it fundamentally affects the performance of ML models. Here, we present a quantitative analysis of time-of-flight secondary ion mass spectrometry (ToF-SIMS) spectra of a simple microarray system of two food dyes using partial least-squares (PLS, linear) and random forest (RF, nonlinear) algorithms. This microarray was generated by a high-throughput sample preparation and analysis workflow for fast and efficient acquisition of quality and reproducible spectra via ToF-SIMS. We drew insights from the bias-variance trade-off, investigated the performances of PLS and RF regression models as a function of training data size, and inferred the amount of data needed to construct accurate and reliable regression models. In addition, we found that the spectral concatenation of positive and negative ToF-SIMS spectra improved the model performances. This study provides an empirical basis for future design of high-throughput microarrays and multicomponent systems, for the purpose of analysis with ToF-SIMS and ML.

Application of Time-of-flight Secondary Ion Mass Spectrometry in Lithium-ion Batteries

Abstract: Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is becoming a powerful tool in the Lithium-Ion Batteries (LIBs) field due to its excellent resolution and sensitivity, as well as its ability to provide spectrally and depth-resolved information. The perspective comprehensively delves into the application of ToF-SIMS in two major areas of LIBs research. Firstly, the article elucidates how ToF-SIMS has been instrumental in deciphering the Solid Electrolyte Interphase (SEI) composition and analyzing electrolyte aging. The insights gleaned from such studies have paved the way for enhancing the longevity and safety of LIBs. Secondly, we explore the role of ToF-SIMS in scrutinizing the distribution of interface reactions, which are critical for understanding charge and discharge mechanisms. The analysis aids in optimizing the interface properties, thereby improving battery performance. Such detections are paramount in ensuring the safety and operational stability of batteries. Overall, the integration of ToF-SIMS in LIBs research offers a promising avenue for the development of advanced and safer energy storage systems.

Photo‐Arbuzov Reactions as a Broadly Applicable Surface Modification Strategy

AbstractChemical vapor deposition (CVD) polymerization is a commonly used approach in surface chemistry, providing a substrate‐independent platform for bioactive surface functionalization strategies. This work investigates the Arbuzov reaction of halogenated polymer coatings readily available via CVD polymerization, using poly(4‐chloro‐para‐xylylene) (Parylene C) as a model substance. Postpolymerization modification of these coatings via catalyst‐free and UV‐induced Arbuzov reaction using phosphites results in phosphonate‐functionalized polymers. The combination of infrared reflection‐absorption spectroscopy (IRRAS), X‐ray photoelectron spectroscopy (XPS), and time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) provides detailed insights into the reaction progress. Time‐dependent studies suggest that the non‐polar phosphites penetrate deep into the CVD films and react with the polymer film. In addition, ToF‐SIMS, scanning electron microscopy (SEM), and atomic force microscopy (AFM) confirm spatial control of the reaction, resulting in localized chemical and topographical surface modification, recognizable by changes in interference color, fluorescence, and wettability. Preliminary 3D fluorescence spectroscopy investigations indicate tunable near‐infrared emission of these polymer films. This work is the first step toward generating multifunctional polymer coatings based on chemically modifiable, CVD polymers with potential applications in biomaterials, sensors, or optoelectronics.

What Elements Really Intercalate into Pd Lattice When Heated in Dimethylformamide?

Palladium hydrides (PdHx) are pivotal in both fundamental research and practical applications across a wide spectrum. PdHx nanocrystals, synthesized by heating in dimethylformamide (DMF), exhibit remarkable stability, granting them widespread applications in the field of electrocatalysis. However, this stability appears inconsistent with their metastable nature. The substantial challenges in characterizing nanoscale structures contribute to the limited understanding of this anomalous phenomenon. Here, through a series of well-conceived experimental designs and advanced characterization techniques, including aberration-corrected scanning transmission electron microscopy (AC-STEM), in situ X-ray diffraction (XRD), and time-of-flight secondary ion mass spectrometry (TOF-SIMS), we have uncovered evidence that indicates the presence of C and N within the lattice of Pd (PdCxNy), rather than H (PdHx). By combining theoretical calculations, we have thoroughly studied the potential configurations and thermodynamic stability of PdCxNy, demonstrating a 2.5:1 ratio of C to N infiltration into the Pd lattice. Furthermore, we successfully modulated the electronic structure of Pd nanocrystals through C and N doping, enhancing their catalytic activity in methanol oxidation reactions. This breakthrough provides a new perspective on the structure and composition of Pd-based nanocrystals infused with light elements, paving the way for the development of advanced catalytic materials in the future.

Utilizing phosphonyl carboxylic acid copolymer as an efficient depressant for flotation separation of chalcopyrite from galena: Experimental and DFT study

The research proposes an innovative galena depressant, known as Phosphonyl carboxylic acid copolymer (POCA), to enhance the efficiency of flotation separation between chalcopyrite and galena. Mineral flotation tests were conducted to investigate the flotation performance of chalcopyrite and galena. The inhibition mechanism of POCA on galena was studied using multiple characterization techniques including Inductively Coupled Plasma Optical Emission Spectrometer (ICP-OES) testing, Zeta potential testing, X-ray photoelectron spectroscopy (XPS) analysis, atomic force microscopy (AFM) testing, contact angle testing, time-of-flight secondary ion mass spectrometry (ToF-SIMS) analysis, and density functional theory (DFT) calculations. In the flotation test, at a concentration of 10 mg/L sodium butyl xanthate (SBX) and pH 9, adding 50 mg/L POCA can reduce the flotation recovery of galena from 83.50 % to below 5 %, whereas the recovery of chalcopyrite was almost influenced. The testing conducted via ICP-OES revealed that POCA promotes the dissolution of Pb2+ from the galena surface. The adsorption of POCA on the galena surface was confirmed through zeta potential testing, XPS testing, contact angle, AFM testing, and ToF-SIMS analysis, it was noted that POCA exhibited high levels of adsorption on the galena surface. Density Functional Theory (DFT) calculations suggest that the chemical interaction between the sulfonic acid present in POCA and the Pb2+ active site of galena is regarded as the primary inhibition mechanism.

Superhydrophobicity wood with reversible photoresponsive property

Superhydrophobic photoresponsive wood (HPW) was synthesized through the vacuum pressure impregnation process with octadecyltrimethoxysilane (OTS), spiropyran, and polyvinyl alcohol (PVA). The process endowed the wood with photostimulation responsiveness and superhydrophobic characteristics. Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS), Fourier transform infrared spectroscopy (FTIR), and a contact angle meter were analyzed to determine the micromorphology, chemical composition, and hydrophobicity of the modified wood. The modified wood had a micro-nanometer mastoid structure at the microscopic level, with a large number of hydrophobic groups. The static water contact angle of the modified wood reached 153°, the water absorption rate decreased from 123.28 % to 19.29 %, and the anti-swelling rate was only 1.69 %, showing good hydrophobic and anti-swelling performance. At the same time, color values of the wood L*, a*, b*, and total color difference ΔE*, it was found that spiropyran made the modified wood have a rapid response to light stimulation.

Electron Donating Functional Polymer Dielectrics to Reduce the Threshold Voltage of n‐Type Organic Thin‐Film Transistors

AbstractLow‐cost and high‐performance electronics based on synthetically simple materials are required to fuel the deployment of smart packaging and wearable electronics. Metal phthalocyanines (MPcs) are promising semiconductors for use in n‐type organic thin film transistors (OTFTs) but often require high operating voltages. The first silicon phthalocyanine‐based OTFT with a polymer dielectric is reported as an alternative to traditional metal oxide dielectrics. Incorporating poly(methyl methacrylate) (PMMA) as the dielectric successfully reduces the threshold voltage (VT) of bispentafluorophenoxy SiPc (F10‐SiPc) from 14.9V to 7.3V while retaining high mobility. Further reduction in VT is obtained by using copolymers and blends of PMMA and dimethylamino ethyl methacrylate (DMAEMA)‐containing polymers, where a higher molar fraction of DMAEMA leads to a consistent drop in VT to ‐0.7 V. The electron‐donating groups of the tertiary amines in the DMAEMA show clear interfacial doping of the semiconductor, reducing the voltage required to populate the dielectric/semiconductor interface with charge carriers and turn on the device. Blending trace amounts of DMAEMA‐containing copolymers with PMMA proves to be an effective strategy for reducing the VT while keeping the charge mobility high, unlike when using pure copolymers with elevated DMAEMA content. Time of flight secondary ion mass spectroscopy (ToF‐SIMS) and X‐ray photoelectron spectroscopy (XPS) demonstrate that the DMAEMA‐containing copolymer is floating to the surface of the PMMA blend at the dielectric–semiconductor interface, which explains the reduced VT. Synchrotron scanning transmission X‐ray microscopy (STXM) demonstrates that PMMA promotes a more edge‐on orientation of F10‐SiPc films, compared to the more face‐on orientation when deposited on the DMAEMA containing copolymer. This study demonstrates a straightforward process for designing dielectric polymers and their blends for the reduction in VT for n‐type OTFTs.

On the way to increase osseointegration potential: Sequential SI-ATRP as promising tool for PEEK-based implant nano-engineering

In the search of the ideal bone implant material, surface initiated atom transfer radical polymerization (SI-ATRP) techniques were successfully employed to modify the polyetheretherketone (PEEK) surface with complex architecture nanolayers featuring hydrophilic poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) or poly(2-hydroxyethyl methacrylate) (PHEMA) branches. As a result, polymer layers with height up to over 300 nm were synthesized to decrease the water contact angle from 92.8° to 23.0°. In-depth analysis of layer topography, structure and elemental composition realized with atomic force microscopy (AFM), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), time-of-flight secondary ions mass spectroscopy (TOF-SIMS) and X-ray photon spectroscopy (XPS) confirmed successful surface modification. Additionally, to demonstrate the applicability of proposed PEEK functionalization, the biomineralization assay in simulated body fluid (SBF) solution was conducted. The high density of hydroxyl and amine groups in branched polymer brushes structure enhanced the rate of hydroxyapatites (HAp) formation substantially. Compared to untreated PEEK, modification with polymer brushes resulted in the creation of cauliflower-like structures with high specific surface area and Ca/P ratio equal to 1.83–1.87 for PEEK grafted with brushes composed of PHEMA backbone segment and PDMAEMA or PHEMA as block polymer branches (PEEK-g-PHEMA-g-PDMAEMA or PEEK-g-PHEMA-g-PHEMA) after 2 weeks. Finally, the process of the hydroxyapatite formation and increase of the layer thickness in a range of 14 days to 6 weeks of immersion in SBF was thoroughly visualized by scanning electron microscopy (SEM).

Direct Visualization of Chemical Transport in Solid-State Chemical Reactions by Time-of-Flight Secondary Ion Mass Spectrometry.

Systematic control and design of solid-state chemical reactions are required for modifying materials properties and in novel synthesis. Understanding chemical dynamics at the nanoscale is therefore essential to revealing the key reactive pathways. Herein, we combine focused ion beam-scanning electron microscopy (FIB-SEM) and time-of-flight secondary ion mass spectrometry (TOF-SIMS) to track the migration of sodium from a borate coating to the oxide scale during in situ hot corrosion testing. We map the changing distribution of chemical elements and compounds from 50 to 850 °C to reveal how sodium diffusion induces corrosion. The results are validated by in situ X-ray diffraction and post-mortem TOF-SIMS. We additionally retrieve the through-solid sodium diffusion rate by fitting measurements to a Fickian diffusion model. This study presents a step change in analyzing microscopic diffusion mechanics with high chemical sensitivity and selectivity, a widespread analytical challenge that underpins the defining rates and mechanisms of solid-state reactions.

Separation and Recovery of Valuable Carbon Components and Li/Ga Metals in Coal Gangue by Using a Flotation Flowsheet.

Coal gangue (CG), an industrial solid waste with high contents of Li and Ga, has attracted the attention of researchers. However, the utilization of CG remains an economic challenge. Pre-enrichment of Li and Ga by flotation was carried out with a view to improving the comprehensive utilization of CG. Mineral composition, time-of-flight secondary ion mass spectrometry (TOF-SIMS), and elemental composition were used to investigate the embeddedness of each mineral and the mode of elemental occurrence in the CG. The results showed that the main mineral compositions of the CG were kaolinite, quartz, and pyrite. Li and Ga were mainly associated with kaolinite and other clay minerals. Li and Ga had a high correlation with Al2O3 and SiO2, while Li and Ga were highly correlated with SiO2/Al2O3, indicating that Li and Ga may be associated with one or more high-alumina minerals. In addition, flotation tests proved that synergistic sorting of ash impurities and valuable components from the CG was a cost-effective method. The ash content of the final product was increased by 3% under the process of prediscarding concentrate-dissociation-secondary flotation, and the contents of Li and Ga in the final product were also slightly enriched, and the recovery rate of the carrier minerals of Li and Ga can reach 66.1%.