Poly(phenylene sulfide amide) (PPSA) has been synthesized by using sulfur as S source which reacts with dichlorobenzamide (DCBA) and alkali in polar organic solvent at the atmospheric pressure. The polymer structures ...Poly(phenylene sulfide amide) (PPSA) has been synthesized by using sulfur as S source which reacts with dichlorobenzamide (DCBA) and alkali in polar organic solvent at the atmospheric pressure. The polymer structures were determined by elemental analysis, FT-IR and H-1-NMR. It is shown that the yielded polymer has linear structure and its structure unit is -p-C6H4-CONH -p-C6H4-S-. The polymer morphology was studied by X-ray diffraction and polarized microscopy. The results show that PPSA is a crystalline polymer and its spherulites are the aggregation of nontwisting lamella or micro-thread structure. Under shearing force, these crystals are dispersed to form micro-fibrillar structure. The decomposition kinetics of PPSA was also studied at different heating rates. The decomposition energy of PPSA is higher than that of PPS.展开更多
A new process for preparing poly(phenylene sulfide amide, PPSA), which is by reaction of sulfur instead of sodium sulfide as S source with dichlorobenzamide (DCBA) and alkali in polar orga...A new process for preparing poly(phenylene sulfide amide, PPSA), which is by reaction of sulfur instead of sodium sulfide as S source with dichlorobenzamide (DCBA) and alkali in polar organic solvent at the atmospheric pressure (called sulfur solution route), is reported in the present paper. The influences of polymerization time, molar ratio of precursors, catalyst and solvent upon the polymer were investigated. To seek the best parameters of polymerization, orthogonal design was employed in the experiments. The results indicate that the molar ratio of precursors is the most significant effect on both of viscosity and yield of the polymer. The suitable parameters for preparing the related polymer are presented. The polymer was characterized by IRspectrum, 1HNMRspectrum and Raman spectrum, etc.展开更多
Poly（phenylene sulfide/ether） （PPSE） was synthesized from 4,4＇-dihydroxydiphenyl sulfide and 4,4＇-dichlorodiphenyl sulfide in solution by nucleophilic substitution reaction. The resulting polymer was characteriz...Poly（phenylene sulfide/ether） （PPSE） was synthesized from 4,4＇-dihydroxydiphenyl sulfide and 4,4＇-dichlorodiphenyl sulfide in solution by nucleophilic substitution reaction. The resulting polymer was characterized by viscosity measurement, elemental analysis, FT-IR, ^1H NMR, X-ray diffraction and thermal analysis. The results showed that the viscosities of the resulting polymer were above 0.68 dL/g, and the linear chain structure of product was confirmed. PPSE had the same reflex indices as poly（p-phenylene sulfide）, an orthorhombic crystalline with unit cell a=0.853, b=0.562, c=1.026nm. The melting temperature, glass transition temperature and initial decomposition temperature were found to be 228℃, 85℃ and 325℃, respectively. The product was soluble in common organic solvents such as NMP, N, N＇-dimethylformamide, N, N＇-dimethylacetamide and 1,2-dichloroethane.展开更多
Commercial poly(p-phenylene sulfide) (PPS) was thermally cured, which resulted in an increase of molecular weight due to cross-linking. Non-isothermal crystallization studies of samples cured for up to 7 days at 250?C...Commercial poly(p-phenylene sulfide) (PPS) was thermally cured, which resulted in an increase of molecular weight due to cross-linking. Non-isothermal crystallization studies of samples cured for up to 7 days at 250?C showed a monotonous increase of crystallization temperature compared to pure PPS. However, a further increase of curing time decreased the crystallization temperature. The change in the half-crystallization time (t1/2) was similar to the crystallization temperature. Thus, the cross-linking of PPS affected crystallization behaviors significantly. To a certain extent, crosslinks acted as nucleation agents, but excessive cross-linking hindered the crystallization. Morphologies observed by polarized optical microscopy suggested that thermal curing for as little as 1 day contributed to the spherulitic structure having a smaller size, that was not observed with pure PPS.展开更多
The morphology of PPTA pulp is investigated by means of optical microscope and scanningelectron microscope (SEM). It shows that PPTA pulp has feather-like branch, needle point-likeend, and irregular cross-section, whi...The morphology of PPTA pulp is investigated by means of optical microscope and scanningelectron microscope (SEM). It shows that PPTA pulp has feather-like branch, needle point-likeend, and irregular cross-section, which are very important for PPTA pulp as a reinforcer. Theseparation limitation of PPTA pulp is also investigated from both torn and brittle break cross-sec-tion. A packing mechanism is proposed to illustrate the microfibril packing in the gel system.展开更多
Poly（phenylene sulfide） （PPS） with different crosslinking levels was successfully fabricated by means of high- temperature isothermal treatment （IT）. The crosslinking degree of PPS was increased with IT time as ...Poly（phenylene sulfide） （PPS） with different crosslinking levels was successfully fabricated by means of high- temperature isothermal treatment （IT）. The crosslinking degree of PPS was increased with IT time as revealed by Fourier-transform infrared spectroscopy and dynamic viscosity measurements. Its influence on the non-isothermal crystallization behaviors of PPS was studied by differential scanning calorimeter （DSC）. The crystallization peak temperature of PPS with 6 h IT was 15 K higher than that of the one with 2 h IT at 30 K/min cooling rate. The non-isothermal crystallization data were also analyzed based on the Ozawa model. The Ozawa exponent m decreased from 3.5 to 2.2 at 232~C with the increase of the IT time, suggestive of intensive thermal oxidative crosslinking reducing the crystallite dimension as PPS crystal grew. The reduced cooling crystallization function K（T） was indicative of the larger activation energy of crosslinked PPS chain diffusion into crystal lattice, resulting in a slow crystal growth rate. Additionally, the overall crystallization rate of PPS was also accelerated with the increase of crosslinking degree from the observation of polarized optical micrograph. These results indicated that the chemical crosslinked points and network structures formed during the high-temperature isothermal treatment acted as the effective nucleating sites, which greatly promoted the crystallization process of PPS and changed the type of nucleation and the geometry of crystal growth accordingly.展开更多
Poly(phenylene sulfide) (PPS) is a well-known organic insulator. However, the PPS thin film, deposited by thermal evaporation in vacuum, showed electrical bistable characteristics. The structure of the PPS thin-film d...Poly(phenylene sulfide) (PPS) is a well-known organic insulator. However, the PPS thin film, deposited by thermal evaporation in vacuum, showed electrical bistable characteristics. The structure of the PPS thin-film device was glass/ITO/PPS (300 nm)/Au. The thin film can be converted to a high conductance state by applying a pulse of 80 V (5 s), and brought back to a low conductance state by applying a pulse of 100 V (5 s). This kind of thin film is potential for active layer of a memory device. The critical voltage of the device is about 40 V, while the read-out voltage is 5 V. We tentatively ascribe the bistable phe-nomenon to the charge transfer from S to C atoms in the PPS molecule chains.展开更多
Achieving low friction and wear of poly(phenylene sulfide)(PPS) without using fillers or blending is a challenging task, but one of considerable practical importance. Here we describe how neat PPS with high tribologic...Achieving low friction and wear of poly(phenylene sulfide)(PPS) without using fillers or blending is a challenging task, but one of considerable practical importance. Here we describe how neat PPS with high tribological performance is achieved by manipulating processing parameters(pressure, flow and temperature). The key to achieving high tribological performance is comparatively high molecular chain orientation, realized in neat PPS, at high shear rates and low pressure. The friction coefficient and wear rate are as low as ~0.3 and~10^(-6) mm^(3)·N^(-1)·m^(-1), respectively, which break the record for neat PPS. These values are even better than those for PPS-based blends and comparable to PPS composites. Further studies show, for the first time, that wear rate decreases exponentially with increasing molecular chain orientation, prompting us to revise the classical Archard's law by including the effect of molecular chain orientation. These findings open the possibility of using neat PPS in highly demanding tribological applications.展开更多
文摘Poly(phenylene sulfide amide) (PPSA) has been synthesized by using sulfur as S source which reacts with dichlorobenzamide (DCBA) and alkali in polar organic solvent at the atmospheric pressure. The polymer structures were determined by elemental analysis, FT-IR and H-1-NMR. It is shown that the yielded polymer has linear structure and its structure unit is -p-C6H4-CONH -p-C6H4-S-. The polymer morphology was studied by X-ray diffraction and polarized microscopy. The results show that PPSA is a crystalline polymer and its spherulites are the aggregation of nontwisting lamella or micro-thread structure. Under shearing force, these crystals are dispersed to form micro-fibrillar structure. The decomposition kinetics of PPSA was also studied at different heating rates. The decomposition energy of PPSA is higher than that of PPS.
文摘A new process for preparing poly(phenylene sulfide amide, PPSA), which is by reaction of sulfur instead of sodium sulfide as S source with dichlorobenzamide (DCBA) and alkali in polar organic solvent at the atmospheric pressure (called sulfur solution route), is reported in the present paper. The influences of polymerization time, molar ratio of precursors, catalyst and solvent upon the polymer were investigated. To seek the best parameters of polymerization, orthogonal design was employed in the experiments. The results indicate that the molar ratio of precursors is the most significant effect on both of viscosity and yield of the polymer. The suitable parameters for preparing the related polymer are presented. The polymer was characterized by IRspectrum, 1HNMRspectrum and Raman spectrum, etc.
文摘Poly（phenylene sulfide/ether） （PPSE） was synthesized from 4,4＇-dihydroxydiphenyl sulfide and 4,4＇-dichlorodiphenyl sulfide in solution by nucleophilic substitution reaction. The resulting polymer was characterized by viscosity measurement, elemental analysis, FT-IR, ^1H NMR, X-ray diffraction and thermal analysis. The results showed that the viscosities of the resulting polymer were above 0.68 dL/g, and the linear chain structure of product was confirmed. PPSE had the same reflex indices as poly（p-phenylene sulfide）, an orthorhombic crystalline with unit cell a=0.853, b=0.562, c=1.026nm. The melting temperature, glass transition temperature and initial decomposition temperature were found to be 228℃, 85℃ and 325℃, respectively. The product was soluble in common organic solvents such as NMP, N, N＇-dimethylformamide, N, N＇-dimethylacetamide and 1,2-dichloroethane.
文摘Commercial poly(p-phenylene sulfide) (PPS) was thermally cured, which resulted in an increase of molecular weight due to cross-linking. Non-isothermal crystallization studies of samples cured for up to 7 days at 250?C showed a monotonous increase of crystallization temperature compared to pure PPS. However, a further increase of curing time decreased the crystallization temperature. The change in the half-crystallization time (t1/2) was similar to the crystallization temperature. Thus, the cross-linking of PPS affected crystallization behaviors significantly. To a certain extent, crosslinks acted as nucleation agents, but excessive cross-linking hindered the crystallization. Morphologies observed by polarized optical microscopy suggested that thermal curing for as little as 1 day contributed to the spherulitic structure having a smaller size, that was not observed with pure PPS.
文摘The morphology of PPTA pulp is investigated by means of optical microscope and scanningelectron microscope (SEM). It shows that PPTA pulp has feather-like branch, needle point-likeend, and irregular cross-section, which are very important for PPTA pulp as a reinforcer. Theseparation limitation of PPTA pulp is also investigated from both torn and brittle break cross-sec-tion. A packing mechanism is proposed to illustrate the microfibril packing in the gel system.
基金financially supported by the National Science Fund for Distinguished Young Scholars (No.50925311)the National Natural Science Foundation of China (No.20976112)
文摘Poly（phenylene sulfide） （PPS） with different crosslinking levels was successfully fabricated by means of high- temperature isothermal treatment （IT）. The crosslinking degree of PPS was increased with IT time as revealed by Fourier-transform infrared spectroscopy and dynamic viscosity measurements. Its influence on the non-isothermal crystallization behaviors of PPS was studied by differential scanning calorimeter （DSC）. The crystallization peak temperature of PPS with 6 h IT was 15 K higher than that of the one with 2 h IT at 30 K/min cooling rate. The non-isothermal crystallization data were also analyzed based on the Ozawa model. The Ozawa exponent m decreased from 3.5 to 2.2 at 232~C with the increase of the IT time, suggestive of intensive thermal oxidative crosslinking reducing the crystallite dimension as PPS crystal grew. The reduced cooling crystallization function K（T） was indicative of the larger activation energy of crosslinked PPS chain diffusion into crystal lattice, resulting in a slow crystal growth rate. Additionally, the overall crystallization rate of PPS was also accelerated with the increase of crosslinking degree from the observation of polarized optical micrograph. These results indicated that the chemical crosslinked points and network structures formed during the high-temperature isothermal treatment acted as the effective nucleating sites, which greatly promoted the crystallization process of PPS and changed the type of nucleation and the geometry of crystal growth accordingly.
基金Supported by the National Natural Science Foundation of China (Grant Nos. 50573039 and 50473009)the National Key Basic Research and Development Pro-gram (Grand No. 2002CB211800)the National Key Program for Basic Re-search of China (Grant No. 2001CCA05000)
文摘Poly(phenylene sulfide) (PPS) is a well-known organic insulator. However, the PPS thin film, deposited by thermal evaporation in vacuum, showed electrical bistable characteristics. The structure of the PPS thin-film device was glass/ITO/PPS (300 nm)/Au. The thin film can be converted to a high conductance state by applying a pulse of 80 V (5 s), and brought back to a low conductance state by applying a pulse of 100 V (5 s). This kind of thin film is potential for active layer of a memory device. The critical voltage of the device is about 40 V, while the read-out voltage is 5 V. We tentatively ascribe the bistable phe-nomenon to the charge transfer from S to C atoms in the PPS molecule chains.
基金financially supported by the National Natural Science Foundation of China (Nos. 21676217, 52003215, 21978240 and 52003219)Youth Project of Basic Research Program of Natural Science in Shaanxi Province (No. 2020JQ179)+1 种基金the Fundamental Research Funds for the Central Universities (Nos. 3102018AX004 and 3102017jc01001)the Open Testing Foundation of the Analytical & Testing Center of Northwestern Polytechnical University (No. 2020T020)。
文摘Achieving low friction and wear of poly(phenylene sulfide)(PPS) without using fillers or blending is a challenging task, but one of considerable practical importance. Here we describe how neat PPS with high tribological performance is achieved by manipulating processing parameters(pressure, flow and temperature). The key to achieving high tribological performance is comparatively high molecular chain orientation, realized in neat PPS, at high shear rates and low pressure. The friction coefficient and wear rate are as low as ~0.3 and~10^(-6) mm^(3)·N^(-1)·m^(-1), respectively, which break the record for neat PPS. These values are even better than those for PPS-based blends and comparable to PPS composites. Further studies show, for the first time, that wear rate decreases exponentially with increasing molecular chain orientation, prompting us to revise the classical Archard's law by including the effect of molecular chain orientation. These findings open the possibility of using neat PPS in highly demanding tribological applications.
