This study optimized the chemical etching conditions of the newly developed UV-polymerized poly(allyl diglycol carbonate) detector DX-22 and evaluated its detection performance. An orthogonal design followed by single-factor experiments was used to investigate the effects of NaOH concentration, etching temperature, and etching time on track morphology, track density, and background counts. The optimal conditions were 6.5 mol/L NaOH, 65 °C, and 8 h. Under these conditions, etched alpha-particle tracks showed clear contours, relatively uniform morphology, predominantly elliptical shapes, low background, and a track density of 201.8 tracks/mm2. CR-39 was used as a reference detector for indoor radon measurements. DX-22 and CR-39 showed consistent spatial track-density trends, with relative area errors of 6.46%-12.93% between fitted response curves. The field comparison was not intended as an absolute radon calibration, and standardized radon-chamber calibration and uncertainty evaluation remain necessary for quantitative dosimetric application. Overall, DX-22 demonstrated promising potential for radon monitoring and radiation protection.
In order to improve the dielectric properties of existing thermosetting resins, taking advantage of reactive fillers is a simple and feasible option. In this paper, we synthesized a new double epoxycyclohexane double-decker silsesquioxane (DEDDSQ), in which the structure of aliphatic epoxy resin introduced into DDSQ successfully, and the resulting structure of DEDDESQ is confirmed by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) spectroscopy, and mass spectrometry (MS). Cyanate ester resin was selected as the case study for the application of DEDDSQ as reactive fillers. A CE/E51/DEDDSQ nanocomposite was fabricated by incorporating a small proportion of E51 resin and DEDDSQ into cyanate ester resin to enhance its comprehensive properties. X-ray diffraction (XRD) and energy-dispersive spectroscopy (EDS) analyses demonstrated that DEDDSQ dispersed uniformly within the resin matrix. Dynamic mechanical analysis (DMA) demonstrated that the CE/E51/8.0DEDDSQ nanocomposites exhibit excellent thermal properties. The glass transition temperature (Tg) of the nanocomposite was measured to be 264 °C, indicating its excellent thermal stability. Dielectric property measurements showed that the addition of DEDDSQ reduced the dielectric constant of the cyanate ester resin, with the CE/E51/8.0DEPOSS nanocomposite exhibiting a dielectric constant of 2.47 at 1 MHz.
In this study, a novel bio-based oxazine resin was synthesized through the reaction of naturally renewable materials: cardanol and furfurylamine. The molecular structure of the target product was confirmed via comprehensive characterization techniques, including Fourier-transform Infrared Spectroscopy (FT-IR), Gel Permeation Chromatography (GPC), Mass Spectrometry (MS), and Nuclear Magnetic Resonance (NMR). Differential Scanning Calorimetry (DSC) revealed that the curing process of cardanol-furfurylamine oxazine (CFZ) exhibited three exothermic peaks (~140, ~240, ~270 °C), which not only helped to optimize the processing conditions but also effectively enhanced the material properties. In the modification experiments, CFZ had been blended and cured with benzoxazine (BZ) at the mass ratios of 2:98, 5:95, 10:90, 20:80, and 40:60. Dynamic Mechanical Thermal Analysis (DMTA) further showed an elevated Loss Factor (tan δ) peak of CFZ-BZ resin, suggesting significantly enhanced toughness. Notably, when the content of the CFZ resin in the composite reached only 5%, the storage modulus achieved its maximum value, highlighting that minimal addition of CFZ resin can optimize the rigidity of the composite, which would drastically reduce material costs and simplify the process. Impact strength testing demonstrated that the impact resistance of CFZ-BZ resin was 6.42 times higher than that of pristine BZ. By integrating renewable materials with rational molecular design, this novel oxazine resin synergistically combines high-temperature resistance, superior toughness, and efficient modification at low loading, positioning it as a promising candidate to replace conventional petroleum-based resins in aerospace, renewable energy, and electronic packaging applications.
Bismaleimide–triazine (BT) resins are widely utilized in various applications, with ongoing efforts to enhance their performance. In this work, a partially epoxidized polyhedral oligomeric silsesquioxane (PEOVS) containing vinyl and epoxy groups was successfully synthesized, and BT/PEOVS nanocomposites were prepared by blending PEOVS with BT resin. The results revealed that the unique structure of PEOVS significantly improved its dispersion within the resin matrix and enhanced the overall properties of the BT resin. The curing mechanism and properties of BT/PEOVS nanocomposites, with weight ratios of 99.5/0.5, 99/1, 98.5/1.5, 98/2, and 96/4, were analyzed using Fourier-transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), X-ray diffraction (XRD), dynamic mechanical analysis (DMA), thermogravimetric analysis (TGA), and dielectric measurements. The addition of PEOVS markedly improved the dielectric performance, with a 2% PEOVS content achieving a dielectric constant of 2.39 and a dielectric loss of 0.0036 at 1 MHz. Furthermore, the glass transition temperature and storage modulus were significantly enhanced, with a PEOVS content of 1.5% resulting in a glass transition temperature of 279 °C. The results demonstrate that incorporating PEOVS, featuring dual reactive functional groups, effectively enhances the comprehensive properties of BT resins, providing valuable insights into their modification and practical applications.
Preparation of high-performance thermosetting resins via bio-based resources is important for the development of a sustainable world. In this work, we proposed the introduction of cyanide structure groups into the molecular structure of epoxy resins to give them excellent heat resistance. A eugenol-based epoxy-phthalonitrile (EEPN) resin was synthesized by a two-step process using the bio-based renewable resource of eugenol, and a series of EEPN/Epoxide resin (E51) blend resins with different EEPN contents were prepared. The structure of the EEPN monomer was characterized and confirmed by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR), and elemental analysis. The thermal stability and dynamic mechanical properties of the cured resins were investigated by thermogravimetric analysis and dynamic mechanical thermal analysis. The experimental results showed that EEPN had excellent heat resistance; the char yield at 800 °C was 67.9 wt%, which was much higher than that of E51 at 26.3 wt%; and the heat resistance of the blended resins was significantly improved with the increase in the EEPN content.
The decay of radon gas in soil and buildings produces alpha radiation, which is the second leading cause of lung cancer in humans. Therefore, by conveniently detecting radon gas in the environment, potential sources of danger can be identified early, and necessary measures can be taken to protect human health. Solid-state nuclear track detectors prepared from polyallyl diglycol carbonate (PADC) resin are the most sensitive detectors for alpha radiation released by radon gas. The traditional method of preparing PADC resin involves free radical thermal polymerization, which suffers from issues such as low polymerization efficiency, long processing time, and the occurrence of defects in the product. In this study, PADC resin was efficiently prepared using a UV initiator. Starting from the polymerization mechanism, experiments were designed using a controlled variable approach, and a rational polymerization apparatus was devised. By comparing the double bond conversion rate, transparency, hardness, and yellowness index of the polymers, the optimal initiator for PADC resin, 2-hydroxy-2-methyl-1-phenyl-1-propanone (1173), was selected. The influence of irradiation intensity, irradiation time, and UV initiator dosage was investigated. The performance of the polymers, including double bond conversion rate, optical properties, dynamic mechanical properties, etching rate, and track detection efficiency, was analyzed. The experimental conditions for preparing PADC resin were optimized: irradiation intensity of 12 mW/cm2, irradiation time of 25 min, and UV initiator dosage of 5 parts. The resulting resin polymer had a double bond conversion rate of 93.2% and a track detection efficiency of 0.714.
This paper presents a composed lithium phosphate (LiPON) solid electrolyte interface (SEI) film which was coated on a lithium electrode via an electrodeposit method in a lithium–sulfur battery, and the structure of the product was characterized through infrared spectrum (IR) analysis, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), environment scanning electron microscope (ESEM), etc. Meanwhile, the electrochemical impedance spectrum and the interface stability of the lithium electrode with the LiPON film was analyzed, while the coulomb efficiency and the cycle life of the lithium electrode with the LiPON film in the lithium–sulfur battery were also studied. It was found that this kind of film can effectively inhibit the charge from transferring at the interface between the electrode and the solution, which can produce a more stable interface impedance on the electrode, thereby improving the interface contact with the electrolyte, and effectively improve the discharge performance, cycle life, and the coulomb efficiency of the lithium–sulfur battery. This is of great significance for the further development of solid electrolyte facial mask technology for lithium–sulfur batteries.
A new type of benzoxazine resin has been synthesized using a natural phenol source, guaiacol, and a biomass amines, furfuramine. The synthesis conditions were optimized; when the reaction molar ratio of guaiacol, furfuramine, and polyformaldehyde was 1:1:4, the highest synthetic yield was reached. The product was characterized via testing using transform infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), mass spectrogram (MS), and nuclear magnetic resonance (1H-NMR) to confirm its molecular structure. A differential scanning calorimetry (DSC) test was conducted to analyze the thermodynamic properties of the product, and the results showed that the product decomposed and evaporated at around 180 °C, making it impossible to achieve self-curing. However, the prepared guaiacol-furfuramine benzoxazine resin (GFZ) can be blended and cured in certain proportions with bisphenol A-aniline oxazine resin (BAZ) as a GFZ/BAZ binary system (5:95, 10:90, 20:80, and 40:60). Dynamic mechanical analysis (DMA) test results showed that when the content of GFZ was 10%, the storage modulus of the copolymer resin was greatly improved. After conducting impact strength tests on the copolymer resin, it was found that the toughness of the copolymer resin had improved, and the maximum impact strength had increased by nearly three times. This indicates that the flexible long-chain structure in GFZ can effectively improve the toughness of the cured copolymer system. The reaction of active groups on benzoxazine molecules with other resins can not only improve the mechanical properties of their cured products, but also has important significance in the preparation of low-cost and environmentally friendly sustainable composite materials with excellent comprehensive performance.
Trisilanolphenyl-polyhedral oligomeric silsesquioxane titanium (Ti-Ph-POSS) was synthesized through the corner-capping reaction, and Ti-Ph-POSS was dispersed in benzoxazine (BZ) to prepare Ti-Ph-POSS/PBZ composite materials. Ti-Ph-POSS could catalyze the ring-opening polymerization (ROP) of BZ and reduce the curing temperature of benzoxazine. In addition, Ti immobilized on the Ti-Ph-POSS cage could form covalent bonds with the N or O atoms on polybenzoxazine, improving the thermal stability of PBZ. The catalytic activity of the Ti-Ph-POSS/BZ mixtures was assessed and identified through 1H nuclear magnetic resonance (1H-NMR) and Fourier-transform infrared (FTIR) analyses, while thermogravimetric analysis (TGA) and dynamic mechanical analysis (DMA) were used to determine the thermal properties of the composite. It was found that PBZ exhibited a higher glass transition temperature (Tg) and better thermal stability when Ti-Ph-POSS was added. The curing behavior of the Ti-Ph-POSS/BZ mixtures showed that the initial (Ti) and peak (Tp) curing temperatures sharply decreased as the content of Ti-Ph-POSS and the heating rate increased. The curing kinetics of these Ti-Ph-POSS/BZ systems were analyzed using the Kissinger method, and the morphology of Ti-Ph-POSS/PBZ was determined via scanning electron microscopy (SEM). It was found that the Ti-Ph-POSS particles were well distributed in the composites. When the content exceeded 2 wt%, several Ti-Ph-POSS particles could not react with benzoxazine and were only dispersed within the PBZ matrix, resulting in aggregation of the Ti-Ph-POSS molecules.
In this paper, the bio-based raw material erythritol was used to introduce an acetal structure into the benzoxazine resins. The benzoxazine-based resins containing an erythritol acetal structure could be degraded in an acidic solution and were environmentally friendly thermosetting resins. Compounds and resins were characterized by 1H nuclear magnetic resonance (1H NMR) and Fourier-transform infrared (FT-IR) analyses, and melting points were studied by a differential scanning calorimeter (DSC); the molecular weight was analyzed by gel permeation chromatography (GPC). The dynamic mechanical properties and thermal stability of polybenzoxazine resins were studied by dynamic mechanical thermal analysis (DMTA) and a thermogravimetric analyzer (TGA), respectively. The thermal aging, wet-heat resistance, and degradation properties of polybenzoxazine resins were tested. The results showed that the polybenzoxazine resins synthesized in this paper had good thermal-oxidative aging, and wet-heat resistance and could be completely degraded in an acidic solution (55 °C DMF: water: 1 mol/L hydrochloric acid solution = 5:2:4 (v/v/v)).
In this study the graphene oxide modified carbonyl iron (GO-CI) was prepared by ?-ray irradiation, which was added to silicone rubber composites to enhance the nuclear radiation shielding performances. X-ray diffraction (XRD) characterization result showed the structure and morphology of the obtained GO-CI nanocomposites. The mixture of GO/CI and the hybrid GO-CI were individually incorporated into the vinyl-terminated polydimethylsiloxane (Vi-PDMS) to prepare referenced SR/GO/CI and SR/GO-CI composites. Compared with SR/GO/CI, the SR/GO-CI exhibited better thermal conduction and mechanical recovery properties. Moreover, the ?-ray radiation shielding ability of SR/GO-CI is much higher than that of pristine SR/GO/CI. CI particles are coated by GO nanosheets to increase surface area to prevent sedimentation of CI. It implies that SR-GO/CI composite would have potential application as the radiation hardening material with thermal conductive and nuclear radiation shielding function.
Preparing biobased high-performance thermoset-ting resins is one of the most important factors for sustainable development. In this work, two kinds of phthalonitrile resins containing spirocycle acetal structures were synthesized from pentaerythritol and renewable vanillin and isovanillin by an efficient two-step process. The structures of vanillin-and isovanillin-based phthalonitrile (VPN and IVPN) monomers were characterized by Fourier transform infrared (FTIR), NMR, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, and elemental analysis. The curing behaviors of these monomers were studied by differential scanning calorimetry and FTIR. The thermal stability and dynamic mechanical properties of the cured resins were investigated by thermogravimetric analysis and dynamic mechanical thermal analysis. The processing properties were studied by a rheological analysis. Compared with traditional petroleum-based phthalonitrile resins such as bisphenol A and bisphenol, cured VPN and IVPN resins exhibited good thermal stability and thermomechanical properties, high glass transition temperature (T-g), and excellent processability.
This paper presents an investigation of the modification of natural oxazines to traditional bisphenol A benzoxazines. Eugenol was reacted with furfurylamine to synthesize a new type of benzoxazine (eugenol–furfurylamine benzoxazine), with a yield of 77.65%; and another new type of benzoxazine (bisphenol A–furfurylamine benzoxazine) was generated from bisphenol A and furfurylamine, with the highest yield of 93.78%. In order to analyze and study the target molecules, IR (infrared radiation) spectroscopy, GPC (gel-permeation chromatograph), mass spectrometry, 1H-NMR (nuclear magnetic resonance), DSC (differential scanning calorimetry), and DMA (dynamic mechanical analysis) tests were conducted. Eugenol-furfurylamine benzoxazine and conventional bisphenol A-aniline benzoxazine (BZ) composite was also analyzed and cured at different mass ratios of 2:98, 5:95, 10:90, 20:80, and 40:60. When the content of eugenol furfurylamine in the blend reached 5%, the strength of the composite was greatly enhanced, while the strength decreased with the increase in eugenol furfurylamine oxazine content. Moreover, octamaleimide phenyl POSS (OMPS, polyhedral oligomeric silsesquioxane) and bisphenol A furamine benzoxazine were mixed at different molar ratios of 1:16, 1:8, 1:4, 1:2, and 1:1. The curing temperature sharply decreased with the increase in OMPS content. When the molar ratio reached 1:1, the curing temperature decreased from 248 to 175℃. A further advantage of using eugenol and furfurylamine is that they are renewable resources, which is important in terms of utilizing resources effectively and developing environmentally friendly products.
采用来源于可再生资源的愈创木酚、癸二胺和多聚甲醛等为原料合成了愈创木酚-癸二胺型苯并嗪单体(G-d),通过红外光谱、凝胶渗透色谱、核磁共振氢谱证明了其分子结构.差热扫描分析和热重分析测试结果表明,其树脂的起始固化温度为225℃,峰值固化温度为246℃.通过热固化工艺得到自固化产物PG-d,并研究其热固化行为、动态力学性能和热分解行为,PG-d的玻璃化转变温度为98.9℃,800℃残碳率为22%.此外,通过基于愈创木酚的苯并嗪G-d与传统双酚A-苯胺型苯并嗪(B-a)按照不同的比例共混形成二元共混体系.当G-d含量为10%时,G-d/B-a体系固化物的冲击强度是B-a均聚体系固化物的3倍以上,表明G-d中的柔性长链结构可有效改善共聚体系固化物的韧性.
In this study a new type of bifunctional epoxy compound (DDSQ-EP) based on double-decker silsesquioxane (DDSQ) was synthesized by process of alkaline hydrolysis condensation of phenyltrimethoxysilane and corner capping reaction with dichloromethylvinylsilane, followed by epoxidation reaction of vinyl groups. The resultant structures were confirmed using Fourier transform infrared spectrometry, nuclear magnetic resonance spectrometry and time-of-flight mass spectrometry, respectively. The DDSQ-EP was incorporated into polybenzoxazine to obtain the PBZ/DDSQ-EP nanocomposites. The uniform dispersion of DDSQ-EP in the nanocomposites was verified by X-ray diffraction and scanning electron microscope. The reactions occurred during the curing of the composites and were investigated using infrared spectroscopy of segmented cures. Dynamic mechanical analysis and thermal gravimetric analysis indicated that the storage modulus, glass transition temperature and thermal stability of PBZ/DDSQ-EP were increased in comparison with pure benzoxazine resins. Assessment of dielectric properties demonstrated that the dielectric permittivity and dielectric loss of polybenzoxazine decreased slightly because of the addition of DDSQ-EP.
The cross-linked imidazolium functionalized anion-exchange membranes is in-situ prepared via reaction of chloromethylated poly(styrene-b-isobutylene-b-styrene) with 1,1?-(1,6-hexanediyl)bisimidazole and N-methylimidazole. The composite membranes of cross-linked imidazolium poly(styrene-b-isobutylene-b-styrene) with a small amount of modified graphene oxide grafted with octadecyl and propyl phenyl imidazolium could be further prepared. These membranes exhibit significantly high chemical stability and ionic conductivity (?), marked by low methanol permeability, together with improved dynamic mechanical properties. The ionic conductivity of cross-linked imidazolium poly(styrene-b-isobutylene-b-styrene) reaches 2.09 x 10-2 S cm- 1 at 80 ?C by introduction of 0.5 wt% loading of modified graphene oxide. This membrane also behaves an excellent chemical stability and ? can remain ca. 82% of the original value after immerged in strong alkaline medium (2 M NaOH) at 60 ?C for 500 h, which is almost the same as that (ca. 82%) of commercial Nafion 115 in acid medium (2 M H2SO4) at 60 ?C for 500 h. The cross-linked imidazolium poly(styrene-b-isobutylene-b-styrene) is characterized as a promising anion exchange membrane materials in fuel cell for its high ionic conductivity, chemical stability and low methanol permeability.
We report on the preparation and characterization of a novel lamellar polypyrrole using an attapulgite–sulfur composite as a hard template. Pretreated attapulgite was utilized as the carrier of elemental sulfur and the attapulgite–sulfur–polypyrrole (AT @400 °C–S–PPy) composite with 50 wt.% sulfur was obtained. The structure and morphology of the composite were characterized with infrared spectroscopy (IR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). An AT @400 °C–S–PPy composite was further utilized as the cathode material for lithium–sulfur batteries. The first discharge specific capacity of this kind of battery reached 1175 mAh/g at a 0.1 C current rate and remained at 518 mAh/g after 100 cycles with capacity retention close to 44%. In the rate test, compared with the polypyrrole–sulfur (PPy–S) cathode material, the AT @400 °C–S–PPy cathode material showed lower capacity at a high current density, but it showed higher capacity when the current came back to a low current density, which was attributed to the “recycling” of pores and channels of attapulgite. Therefore, the lamellar composite with special pore structure has great value in improving the performance of lithium–sulfur batteries.
Designing novel low-melting, high-rigidity phthalonitrile resin is of great significance in the current context of development. In this study, rigid spirocycle acetal structure was introduced into phthalonitrile to reduce the melting point and maintain their thermal stability. The chemical structure of resins was confirmed by nuclear magnetic resonance (NMR) spectrometry, matrix-assisted laser desorption/ionization time of flight (MALDI-TOF) mass spectrometry and Fourier-transform infrared (FTIR) spectroscopy. The curing behaviors were studied by differential scanning calorimetry (DSC). Thermal stability and mechanical properties of the cured resins were investigated by dynamic mechanical thermal analysis (DMTA) and thermogravimetric analysis (TGA). The processability was studied by rheological analysis. The results indicated the three monomers had a low melting temperature, wide processing windows and low viscosities. These polymers did not exhibit Tg from room temperature to 400°C, exhibited superb dynamic mechanical property and thermal stability.
Preparation of optically active polymer particles constructed by chiral helical disubstituted polyacetylenes via precipitation polymerization.
退役硅橡胶复合绝缘子的合理处置是电力行业需要解决的重要问题.利用硅烷偶联剂表面处理退役硅橡胶绝缘子胶粉,再将其填充室温硫化硅橡胶.利用红外光谱和热失重(TGA)分析表面处理效果,利用万能材料试验机、TGA、动态力学热分析和扫描电镜对硫化胶性能和结构进行分析.结果 表明,硅烷偶联剂可有效地对退役硅橡胶复合绝缘子胶粉进行表面改性,其中乙烯基三乙氧基硅烷是较佳的偶联剂;在5~35份改性胶粉用量范围内,所得硫化胶拉伸强度提高7%~23%;填充处理胶粉不影响硫化胶的玻璃化转变温度(-27~-23℃),提高了硫化胶最大热分解速率温度(最高达到532℃)和模量(30℃模量提高7%~85%),且在基体内分散均匀.因此,退役硅橡胶复合绝缘子胶粉作为室温硫化硅橡胶的填充材料是实现其回收再利用的有效途径.