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NEW JOURNAL OF CHEMISTRY · 2019 ·Vol. 44 ·期 4 ·1236-1244 · IF 3.069

Preparation of graphene via wet ball milling and in situ reversible modification with the Diels–Alder reaction

Jianfeng Xu,Xiaomin Zhao,Feixiang Liu,Lun Jin,Guohua Chen

Functionalized graphene (G-MA) was prepared by a facile wet ball milling strategy, which achieved exfoliation and functionalization of graphite simultaneously. The G-MA showed excellent dispersion in water and polar solvents. Thus, a G-MA coating was prepared from G-MA in mixed solvents (H2O–ethanol) without binder or surfactant. The scanning electron microscope (SEM) images of the G-MA coating exhibited a smooth and flat surface. The G-MA coating showed a conductivity of 769 S m−1 at room temperature, and a big increase could be found at 2000 S m−1 after thermal treatment under 200 °C for 2 h, indicating the restoration of the conjugated structure via the reverse Diels–Alder reaction. This synthetic method of functionalized graphene offers a powerful strategy for the reversible modification of the graphene electronic properties, which may expand their usage.

CAS / MDL: 108-31-6 1310-73-2
研究领域: 材料科学 · 化学工程
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Tungsten · 2025 · IF 11.2

Extraction and response surface methodology optimization of tungsten and molybdenum from spent fluidized catalytic cracking catalysts

Zhao Jian-Ying,Mu Pan-Pan,Liu Hao,Chachina Svetlana B.,Zhang Xiao-Guang,Zhang Shao-Gang,Pan Dean

Waste fluidized catalytic cracking (FCC) catalysts contain strategic metals with high recycling value, and effective treatment of these waste catalysts is crucial for resource recovery and environmental protection. In this study, a leaching process of “oxidation treatment–alkali roasting–wet mill leaching” was proposed for the extraction of tungsten (W) and molybdenum (Mo) valuable metals from spent FCC catalysts, and a technological pathway suitable for industrial production was explored through a detailed investigation of the conversion mechanism and process optimization. After the pretreatment by oxidation and roasting at 600 ℃ for 4 h, the optimal conditions for alkali roasting were found to be 950 ℃ with the addition of three times the theoretical amount of alkali (Na 2 CO 3 ), which ensured full conversion and avoided the generation of impurities. Through one-factor exploration and response surface optimization, the average leaching rate for W and Mo reached 87.23% and 99.50%, respectively, under the wet mill leaching conditions of a 200-mesh particle size, liquid–solid ratio of 2.79, a wet milling time of 1.18 h, a pellet ratio of 6.44:1, and a roasting time of 114.61 min. It was observed that both heating leaching and wet mill leaching could achieve full extraction with a relatively small liquid–solid ratio, thereby minimizing the production and discharge of waste liquid. The formation of nickel tungstate (NiWO 4 ) was identified as the main factor limiting the leaching of W, and it was found that increasing the oxygen content during the roasting process could improve the leaching efficiency. This study provides practical guidance and a scientific basis for the environmentally friendly and resource-efficient utilization of spent FCC catalysts.

CAS / MDL: 497-19-8
研究领域: 冶金工程 · 环境科学 · 资源回收
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JOURNAL OF THE AMERICAN CERAMIC SOCIETY · 2022 ·Vol. 106 ·期 1 ·274-284 · IF 4.186

Influence of dry- and wet-milled LLZTO particles on the sintered pellets

Hongpeng Zheng,Guoyao Li,Hezhou Liu,Yongmin Wu,Huanan Duan

A Ta-doped Li 7 La 3 Zr 2 O 12 (LLZTO) solid electrolyte is a promising candidate for all-solid-state lithium battery due to its high ionic conductivity and stability against lithium metal. In this work, physicochemical properties of both dry- and wet-milled LLZTO particles were investigated. Based on X-ray diffraction, Fourier transform–infrared, thermogravimetric analysis, and scanning electron microscopy results, it was confirmed that highly reactive LLZTO powder prepared in dry milling conditions exhibited faster size reduction, rougher surface morphology, fewer surface impurities, and less agglomerated particles, in contrast to those in wet milling conditions. Sintering these dry-milled powders at 1320°C for 10 min in the air via solid-state reaction produced dense ceramic pellets with a relative density of 97.4%. The room-temperature ionic conductivity for LLZTO pellet via the dry milling was determined to be 6.94 × 10 −4 S cm −1 . Li–sulfur batteries based on the pellets showed an initial discharge capacity of 1301 mA h g −1 and a coulombic efficiency of 99.82% when cycled at room temperature. The effect of the milled powder on the sintered pellets was discussed in terms of boundary mobility, pore mobility, and morphology.

CAS / MDL: 1314-61-0
研究领域: 材料科学 · 电化学
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FOOD HYDROCOLLOIDS · 2024 · IF 11

Mechanical (ball milling) activation to regulate microstructure of κ-carrageenan and improve freeze-thaw stability of κ-carrageenan gels and κ-carrageenan-based emulsion gels

Xinwei Xu,Yating Ding,Huifen Weng,Qiong Xiao,Jun Chen,Yonghui Zhang,Qiuming Yang,Fuquan Chen,Anfeng Xiao

To expand the wide range of applications of κ-carrageenan in the food and biomedical fields, we have physically modified the carrageenan and focused on its freeze-thaw stability. In this study, κ-carrageenan (KC) was modified by mechanically activated to prepare wet ball milling κ-carrageenan (WMKC), and its properties were determined. The research results indicate that mechanical activation helps improve the freeze-thaw stability of KC gels and enables KC to better maintain its gel network structure during the freeze-thaw process. These phenomena are related to the effects of mechanical activation on the particle morphology, molecular structure, molecular interactions, and moisture migration of κ-carrageenan. The particle morphology images demonstrated that the WMKC particles exhibited a more irregular surface, which facilitated greater penetration of water molecules into the interior of the κ-carrageenan particles. Furthermore, the results of molecular structure and molecular interaction analyses showed that mechanical activation resulted in the removal of sulfate groups from the κ-carrageenan molecular chain. This resulted in more free -OH being exposed on the molecular chain, which in turn provided more binding sites for KC molecules with water molecules. Low-field nuclear magnetic resonance (LF-NMR) results also proved that WMKC could better maintain the binding with water molecules during the freeze-thaw process. A better combination of WMKC molecules and water molecules can significantly diminish the irreversible damage to the gel network structure of WMKC during the freeze-thaw process, thereby effectively enhancing the freeze-thaw stability of WMKC. In addition, we further used WMKC as the gel matrix and investigated that the freeze-thaw stability of the WMKC-based emulsion gel was optimal when the mechanical activation duration was 3h, which well meets the demand of κ-carrageenan emulsion gels in the frozen food industry.

CAS / MDL: 7758-02-3
研究领域: 食品科学 · 生物材料学
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FOOD HYDROCOLLOIDS · 2020 · IF 7.053

Wet media planetary ball milling remarkably improves functional and cholesterol-binding properties of okara

Tao Yang,Hui-Ling Yan,Chuan-He Tang

The utilization of okara , an important byproduct of soybean industry, has attracted increasing interests, due to its good nutrition and potential health effects. This work investigated the influence of a wet media planetary ball milling on some physicochemical and functional properties and cholesterol binding capacity (CBC) of okara from defatted soy flour . The tested properties included particle size, ζ -potential, water holding and swelling capacities (WHC and WSC), oil binding capacity (OBC), cation exchange capacity (CEC), emulsifying ability and emulsion stability indices (EAI and ESI), foaming ability (FA) and foam stability (FS). The results indicated that a milling with increasing time from 5 to 15 h resulted in a progressive decrease in z -average diameter (up to 270 nm) of okara particles, and thus improved their water dispersibility. In general, the milling progressively increased WHC , WSC, OBC, CEC, EAI, FA and CBC, in a milling time dependent way. Especially for the okara milled for 15 h, its EAI became comparable to that of soy protein isolate (SPI), while its ESI was considerably higher than SPI. The CBC of okara at pH 7.0 increased by 3-folds, after the milling for 15 h. Such improvements of functionalities were largely attributed to the transformation of insoluble components into water-dispersible, highly functional colloidal nanoparticles , as well as disruption of crystalline polysaccharides for milled okara. The findings are of interest not only for guiding the highly-added-value utilization of okara, but also for the development of a kind of highly functional and health-benefiting food functional ingredients with a great potential to be applied in food formulations.

研究领域: 食品科学 · 营养学
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CARBON · 2025 · IF 11.6

LiCl modified graphene by wet ball-milling strategy for high performance lithium-ion battery

Wei Wu,Ranlu Zheng,Yixuan Bai,Qingyi Feng,Bo Li,Yongliang Tang,Hongxiang Deng,Xiaotao Zu,Shuangyue Wang,Xia Xiang

Graphene-based lithium-ion batteries suffer from the poor initial coulombic efficiency and low mass loading. A convenient method is proposed to replenish the Li loss in the first cycle and improve the cycling stability of high mass loading batteries simultaneously in this work. Graphene is modified by introducing LiCl (G/LC) through a wet ball-milling process, which leads to the formation of hybrid solid electrolyte interface. As a result, the half-cells based on high mass loading G/LC electrodes exhibit obviously improved initial coulombic efficiency (>90 %) and high areal specific capacity of 2.53 mAh cm −2 at high current density of 0.55 mA cm −2 . Furthermore, the full-cells based on G/LC anode paired with LiNi 6 Mn 2 Co 2 O 2 cathode deliver a high initial coulombic efficiency of 76.7 %, as well as a high-capacity retention of 97.52 % after 200 cycles, suggesting the potential application of this extend strategy for rechargeable batteries.

CAS / MDL: 64-17-5 7447-41-8
研究领域: 材料科学 · 能源存储
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IONICS · 2020 ·Vol. 26 ·期 7 ·3267-3274 · IF 2.394

Investigation of wet-milled graphene nanosheets with sulfur doping for lithium-ion battery

Guo Binbin,Ananth K. Prem,Zhang Jingshi,Ji Xinzhu,Bai Jiaming

In this work, sulfur-doped graphene nanosheets (SGNS) were fabricated by wet ball milling pristine graphite with carbon disulfide (CS 2 ). With the presence of liquid CS 2 , pristine graphite was easily infiltrated and exfoliated to graphene nanosheets, and sulfur atom was successfully doped onto the surface of graphene nanosheets. The as-prepared SGNS with sulfur doping content (12.49 wt.%) showed higher reversible specific capacity (588.2 mAh g −1 and 266.2 mAh g −1 ) than the commercial graphite (240 mAh g −1 and 69.7 mAh g −1 ) at current densities of 100 and 1000 mA g −1 , respectively. This method described in this study can provide a simple and low-cost strategy for the preparation of SGNS as a promising anode material for lithium-ion batteries.

CAS / MDL: 75-15-0
研究领域: 材料科学 · 能源存储
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CERAMICS INTERNATIONAL · 2020 ·Vol. 46 ·期 16 ·24799-24804 · IF 3.83

One-step synthesis of ZrO2 nanopowders dispersed with graphene by ball milling

Pengfei Pan,Xu Wang,Yaqi Ji,Wumei Dong,Lei Zhang,Ling Wang,Ming Zhang

A simple, efficient and low-cost method to synthesize zirconia nanopowders dispersed with graphene by wet ball milling was reported in this paper. The raw material for ball milling is cheap graphite powder rather than expensive graphene. Graphite powders were exfoliated into graphene nanosheets (GNSs) in the process of ball milling, as a result of strong shear forces and moderate impact forces between graphite powders, milling balls, and ZrO 2 nanoparticles . The mixed powders were milled for 3, 10, 20, 30, 40, and 50 h, respectively. Moreover, the morphology, composition and structure of the mixed powders milled were characterized by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy , Fourier transform infrared spectroscopy , and field emission transmission electron microscopy . Results showed that the graphite powders were exfoliated effectively, and the GNSs were dispersed uniformly in the zirconia simultaneously. The presence of zirconia nanoparticles significantly improved the efficiency of ball milling exfoliation.

研究领域: 材料科学 · 纳米技术 · 无机非金属材料 · 复合材料
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Foods · 2024 ·Vol. 13 ·期 4 ·624 · IF 4.7

Emulsification Characteristics of Insoluble Dietary Fibers from Pomelo Peel: Effects of Acetylation, Enzymatic Hydrolysis, and Wet Ball Milling

Kuimin Yang,Jieqiong Yao,Kaixin Shi,Chenxi Yang,Yang Xu,Peipei Zhang,Siyi Pan

To improve the application potential of pomelo peel insoluble dietary fiber (PIDF) in emulsion systems, acetylation (PIDF-A), cellulase hydrolysis (PIDF-E), and wet ball milling (PIDF-M) were investigated in this paper as methods to change the emulsification properties of PIDF. The impact of the methods on PIDF composition, structure, and physicochemical properties was also assessed. The results demonstrated that both acetylation modification and cellulase hydrolysis could significantly improve the emulsification properties of PIDF. The emulsions stabilized with PIDF-A and PIDF-E could be stably stored at 25 °C for 30 d without phase separation at particle concentrations above 0.8% (w/v) and had higher storage stability: The D4,3increments of PIDF-A- and PIDF-E-stabilized emulsions were 0.98 μm and 0.49 μm, respectively, at particle concentrations of 1.2% (w/v), while the storage stability of PIDF-M-stabilized emulsion (5.29 μm) significantly decreased compared with that of PIDF (4.00 μm). Moreover, PIDF-A showed the highest water retention capacity (21.84 g/g), water swelling capacity (15.40 mL/g), oil retention capacity (4.67 g/g), and zeta potential absolute (29.0 mV) among the PIDFs. In conclusion, acetylation modification was a promising method to improve the emulsifying properties of insoluble polysaccharides.Keywords:pomelo peel insoluble dietary fiber;acetylation;cellulase hydrolysis;wet ball milling;emulsifying properties

CAS / MDL: 9032-08-0 9000-90-2
研究领域: 食品科学 · 化学工程 · 材料科学
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FOOD HYDROCOLLOIDS · 2025 · IF 12.4

Wet ball-milling fabricated deacetylated chitin nanofibers for meat saltiness enhancement

Jing Liao,Xingyue Zhao,Yuhang Zhou,Jiamin Zhang

The reduction of salt usage in meat products is of significant interest to the meat processing industry. In this context, chitin nanofibers (ChNFs) have emerged as a potential candidate for reducing salt usage in meat products. In this study, deacetylated chitin nanofibers (D-ChNFs) with varying degrees of deacetylation (DDs) were prepared by subjecting native chitin to a partial deacetylation process, followed by a wet ball-milling treatment. The fabricated D-ChNFs were characterized and used as saltiness enhancers for pork fillets. The enhanced saltiness mechanism was elucidated by exploring the interaction between ChNFs and Cl − . The results have shown that when DD is increased from 5.9 % to 28.6 %, D-ChNFs with a more dispersed nanostructure can be obtained, with a diameter range of 10–30 nm and a length of several microns. Furthermore, the pork fillets cured with D-ChNFs exhibited higher saltiness values compared to the control groups, and the optimal perceived saltiness was obtained when the ChNF-12 (DD = 28.6 %) was added. Quantum chemical calculation results demonstrated that the interaction intensity between Cl − and the functional groups on the D-ChNFs is in the order of -NH 3 + /−OH > -NH 3 + >-NHCOCH 3 . D-ChNFs can bind Cl − to their surface through electrostatic attraction as the dominant force, and scale up the proportion of Na + on the meat surface that can bind to taste receptor cells, thus enhancing the meat saltiness. The findings of this study provide a theoretical basis for the development of novel salt reduction methods in meat industry.

CAS / MDL: 7647-14-5
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JOURNAL OF MATERIALS SCIENCE · 2025 · IF 3.9

Scalable synthesis and performance optimization of silicon/ flake Graphite@Hard carbon composite anodes for lithium-ion batteries by wet ball milling

Yukun Zhang,Fang Ke,Zijing Zheng,Shuai Zhang,Qingyong Duan,Hepeng Lu,Shanxin Xiong,Xiaoqin Wang,Jinhang Li

With the saturation of lithium-ion battery cathode materials research, anode materials have gained increasing attention for their potential advancements. Among them, silicon electrodes, with a theoretical capacity nearly ten times that of graphite, face challenges from significant volume expansion during the charge–discharge cycle, leading to capacity fading and reduced cycle life. Therefore, this study shows a scalable and economical approach. Firstly, silicon anodes were improved through the preparation of silicon/graphite composites via wet ball milling. Subsequently, the phenolic resin was used as a coating and sintered to create a robust carbon layer, which serves to strengthen the composite structure and reduce the volume expansion of silicon. The composite was prepared with 800 mesh flake graphite, silicon-carbon ratio 1:2, ball milling for 5 h and coated with hard carbon (Si/FG@HC-800-125) shows remarkable electrochemical performance, reaching an initial discharge specific capacity of 1024.5 mAh/g and an initial Coulombic efficiency of 86.9%, with a capacity retention rate of 62.92% after 200 cycles. The findings show that the combination of wet ball milling and hard carbon coating effectively enhances the conductivity and structural stability of silicon-based anodes, providing a viable route for large-scale production.

CAS / MDL: 108-46-3
研究领域: 材料科学 · 储能 · 电化学 · 纳米材料 · 电池技术
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