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1.
To tailor a new electromagnetic wave (EMW) absorbing material with lower reflection coefficient (RC) and larger operating frequency band, the CVD Si3N4–SiCN composite ceramics were prepared from SiCl4–NH3–C3H6–H2–Ar system and then annealed at the temperatures of 1400–1700°C in N2 atmosphere. Effect of the annealing temperatures on the microstructure, phase composition, permittivity, and microwave‐absorbing properties of the ceramic were investigated. Results showed that the CVD Si3N4–SiCN ceramics gradually crystallized into nanosized SiC grains, Si3N4 grains and graphite (T ≤ 1600°C), and then the grains grew up at T = 1700°C. The permittivity, dielectric loss, and electrical conductivity of as‐annealed CVD Si3N4–SiCN ceramics (T ≤ 1600°C) increased firstly due to the formation of conductivity and polarity network and the increase in nanograin boundary, and then decreased at 1700°C because of the growth of nanograins and the disappearance of nanograin boundary. The minimal RC and effective absorption bandwidth of the as‐annealed CVD Si3N4–SiCN ceramic at 1600°C was ?41.67 dB at the thickness of 2.55 mm and 3.95 GHz at the thickness of 3.05 mm, respectively, demonstrating that the totally crystallized CVD Si3N4–SiCN ceramic (T = 1600°C) had the superior microwave‐absorbing ability.  相似文献   

2.
In the high‐temperature ternary perovskite piezoelectric system xPbTiO3yBiScO3zBi(Ni1/2,Ti1/2)O3 (PT–BS–BNiT), the addition of bismuth to the A site and nickel to the B site leads to compositions that exhibit diffuse relaxor‐like behavior. For these, depolarization temperature, not Curie point, is the critical value of temperature. Depolarization temperature (Td) is defined as the temperature at which the steepest loss in polarization occurs. This temperature is observed in poled materials through two different methods: loss tangent measurements and in situ d33. Across the ternary system, multiple dielectric anomalies occurred which was observed in dielectric tests where the dielectric peak broadens and becomes frequency dependent as BNiT content increased. For different compositions, the value of Td ranged between 275°C–375°C. Values for the piezoelectric coefficient increased with temperature up to d33 = 1000 pC/N during in situ d33. High temperature (up to 190°C) and high field (up to 40 kV/cm) were also applied to test ferroelectric properties in these regimes.  相似文献   

3.
Unidirectional (UD) composite laminates based on carbon fibers (CF) and high-performance polyethylene fibers (PEF) were prepared with partially polymerized methyl methacrylate (MMA) at 25°C, followed by heating at 55°C (well below the softening point of PEF) for 2 h. The viscoelastic behavior of the composite was studied through dynamic mechanical analysis at different volume fractions of the fibers. Several parameters such as the storage modulus (E′), loss modulus (E′), and loss factor or damping efficiency (tan δ) were determined between 40 and 160°C in a resonant frequency mode. The glass transition temperature (Tg) increased to a higher region with increase in the volume of PEF in the hybrid laminates. It was also observed that the efficiency of the composite decreases with increase in the volume fraction of the fibers. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 67:1631–1637, 1998  相似文献   

4.
The effect of thermal treatment over a wide range of temperature (130–280°C) on the crystallization behavior of nylon 6 was studied by using DSC, FTIR, and polarized light microscope equipped with a hot stage. The crystallization and the subsequent melting behavior of the nylon 6 samples treated at different temperatures (Ts) were classified into four types. When Ts was higher than 236°C or lower than 213°C, the crystallization behavior of nylon 6 was insensitive to the variation of Ts. When Ts was in the range of 213–235°C, the crystallization behavior was sensitive to the change of Ts. The polarized light microscopic experiments have demonstrated that a large amount of tiny ordered nylon 6 segments/cluster persisted when nylon 6 film are heated to 231°C. Consequently, the fastest crystallization speed was observed. As Ts was between 214 and 223°C, both the Tm and the ΔHm were higher than those of the nylon 6 samples treated at other temperature. The polarized light microscopic investigations have also demonstrated that molten nylon 6 crystallizes by using the un‐molten nylon 6 crystals as nucleation center at 220°C. Crystallization at higher temperature produces nylon 6 with thicker crystalline lamella. The above results are helpful for rational design of thermal treatment procedure to obtain nylon 6 with different crystalline features. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42413.  相似文献   

5.
The organic–inorganic hybrid boron‐containing phenol–formaldehyde (BPFR) resin/SiO2 nanocomposites was synthesized in‐situ from boric acid, phenol, and tetramethoxysilane. The structure of BPFR modified and the distributions of silicon element were studied by Fourier‐transform infrared spectroscopy, energy dispersive X‐ray spectrometry, and transmission electron microscope, respectively. The glass transition temperature (Tg) was determined by torsional braid analysis. The results show that silicon element distribution is homogeneous, and the size of nanosilica is about 40–60 nm. The thermal stability and kinetics parameters of thermal degradation were determined by thermogravimetry analysis (TGA). TGA results show that the resin modified has higher heat resistance property when the additive quantity of SiO2 was 3 wt%. The temperature of 5% weight loss is 487.7°C, which is 12.4°C higher than that of common BPFR. The residual ratio of 3 wt% SiO2/BPFR was 62.3% at the temperature of 900°C, which is 11.2% higher than that of common BPFR. The mechanics loss peak Tp of 3% SiO2/BPFR is 33°C higher than common BPFR. Fiberglass‐reinforced BPFR modified by 3 wt% SiO2 has better mechanical and dielectric properties than that of common BPFR. POLYM. COMPOS., 2008. © 2007 Society of Plastics Engineers  相似文献   

6.
Poly(glycolide‐co‐l ‐lactide) (PGA/PLLA) is a random copolymer with 92 wt % PGA, being the basic resin for Vicryl® suture. Molecular dynamics of PGA/PLLA in its wholly amorphous state and during isothermal cold crystallization at 70 and 80°C have been analyzed. Experimental results were generated over a wide range of frequency and temperature by broad‐band dielectric spectroscopy (DRS). The variation of the average relaxation time (defined as τ = [1/2]πfmax where fmax is the frequency at maximum loss for the main α relaxation) has been studied during cold crystallization and the temperature dependence of this average relaxation time for wholly amorphous and crystallized samples has been analyzed. This behavior has been modeled by Havriliak–Negami, Vogel–Fulcher–Tammann, and Kohlrausch–Williams–Watts equations. The evolution profile of the dynamics (frequency at which the maximum loss appears, fmax) depends on the crystallization temperature, being different at 80°C relatively to 70°C, which could reflect different progress of the spherulitic morphology, as it is shown by the evolution of the morphologies obtained during the crystallization processes, followed by optical microscopy. While the loss maximum (and consequently relaxation times) remains almost unmodified during the crystallization process at 70°C, for the process at 80°C the maximum first moves slightly to higher frequencies (shortening of relaxation times) and at the final stages of crystallization it moves to lower frequencies (increasing the relaxation times). Supporting evidence about the thermal behavior of the polymers has been obtained with DSC. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007  相似文献   

7.
Stability, including thermal stability, conductivity stability in air and after thermal treatment (100–200°C), of the polyaniline (PANI) films synthesized by a doping–dedoping–redoping method was investigated. It was found that thermogravimetric analysis (TGA) curves undergo three steps: loss of water or solvent, dedoping and decomposition, and those depend on the counterions. Compared with PANI films doped with camphor sulfonic acid (CSA) in m‐cresol, the thermal stability of the doped PANI films is improved by the new method, and thermal stability in the order of PANI–H3PO4 > PANI–p‐TSA > PANI–H2SO4 > PANI–HCl, PANI–HClO4 > PANI–CSA was observed. The conductivity of the doped PANI films at room temperature was reduced after thermal treatment, and it is dependent of the counterions. It was found that the conductivity stability of PANI–p‐TSA and PANI–CSA is the best below 200°C. When the doped PANI films were placed in air, their conductivity decrease slowly with time due to deproton, and also depends on the counterions. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 615–621, 1999  相似文献   

8.
The relaxation behavior of polyimide and its nanocomposite containing 10 wt % of graphene was studied by using the dynamic mechanical spectrometer. Dynamic mechanical analysis of polyimide and its composite was performed as a function of temperature and frequency in the temperature range of 25–480 °C and frequency range between 0.05 and 100 Hz. The effect of increasing frequency of testing from 0.05 to 100 Hz is a significant shift from the glass transition temperature, Tg, to higher temperature from 360 °C at 0.05 Hz to 420 °C at 100 Hz. The tan δ peak height for both α and β transitions decreased with increasing test frequency from 0.24 at 0.05 Hz to 0.08 at 100 Hz, due to increasing restriction to chain motion. At any given testing frequency, the Tg for the composite was shown to be higher than that for the matrix by about 5–10 °C. The Arrhenius equation was used to calculate the activation energy for both α and β transitions. The activation for α and β transitions for the composite and polyimide matrix were determined to be 688 and 537 kJ/mol and 313 and 309 kJ/mol, respectively, indicating that a significant increase in the energy barrier to chain relaxation occurred as a result of reinforcement of polyimide with low weight fraction of graphene. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43684.  相似文献   

9.
Ternary compositions based on Bi(B′B″)O3–PbTiO3‐type compounds have been investigated for high‐temperature piezoelectric applications. Compositions in the ternary were chosen to be near the binary morphotropic phase boundary (MPB) composition of BiScO3–PbTiO3 (BS–PT). Ternary compositions in (100?x?y)BiScO3–(x)Bi(Zr0.5Zn0.5)O3–(y)PbTiO3 [(100?x?y)BS–xBZZ–yPT] have been investigated with x ≤ 7.5. For compositions with x > 10, the Curie temperature (TC) decreased below 400°C. Dielectric, piezoelectric, and electromechanical properties were characterized as a function of temperature, frequency, and electric field. Small additions of BZZ were shown to increase the electromechanical properties with only a small loss in TC. The electromechanical properties were temperature stable up to the depoling temperature. The most promising composition exhibited a TC of 430°C, piezoelectric coefficient (d33) of 520 pC/N, and a planar coupling factor (kp) of 0.45 that remained unchanged up to depoling temperature at 385°C.  相似文献   

10.
The heat‐resistant copolymer of N‐phenylmaleimide (NPMI)–styrene (St)–maleic anhydride (MAH) was synthesized in xylene at 125°C with di‐tert‐butyl diperoxyterephthalate as an initiator. The characteristics of the copolymer were analyzed by Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy (1H‐NMR and 13C‐NMR), gel permeation chromatography, and elemental analysis. The 13C‐NMR results show that the copolymer possessed random sequence distribution; this was also supported by the differential scanning calorimetry experiment, in which a single glass‐transition temperature (Tg) of 202.3°C was observed. The thermal stability and degradation mechanism of the copolymer were investigated by thermogravimetric analysis. Using the Kissinger equation and Ozawa equation, we proved a nucleation controlling mechanism with an apparent activation energy of 144 kJ/mol. Blends of acrylonitrile–butadiene–styrene with the NPMI–St–MAH copolymer with various contents were prepared with a twin‐screw extruder processes. The mechanical and thermal properties of the materials, such as the tensile and flexural strength, Tg's, and Vicat softening temperatures, were all enhanced with the addition of the modifier, whereas the melt flow index decreased. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012  相似文献   

11.
The mechanical properties, tensile strength, and elongation were investigated for poly(vinyl chloride) (PVC) samples mixed with dioctylphthalate (DOP) at concentrations from 0 to 100 parts per hundred parts PVC at 23°C. It was found that the tensile strength decreased with the increase of concentration, and the elongation was increased until a concentration of 30 DOP content, and then decreased. This leads to the suggestion that intermolecular plasticization is dominant until 30 DOP content, while interstructural plasticization is prevailing for higher concentrations. The permittivity ε′ and the dielectric loss factor ε″ of the same samples have been measured in the frequency range 102–105 Hz at temperatures from 3 to 96°C. Results show that as the DOP content increases in PVC, the dielectric absorption becomes broader, and the glass transition temperature Tg is lowered. The magnitude of the loss peak decreases with an increase of DOP content to a minimum at concentrations from 40 to 60 DOP content. At higher concentrations the loss peak is increased and Tg is unaltered. Another absorption was observed at 100 Hz and at high temperatures, which was attributed to Maxwell–Wagner effect or direct current conductivity or both of them. It was found that the sample containing 40 parts DOP in 100 parts PVC possesses the best mechanical and electrical properties.  相似文献   

12.
The dielectric relaxation behavior of different conducting carbon black‐filled ethylene‐octene copolymer (EOC) vulcanizates prepared by melt‐mixing method has been studied as a function of frequency (100 Hz–5 MHz) over a wide range of temperatures (25–100°C). The effect of filler loading and frequency on AC conductivity, dielectric permittivity, impedance, and dielectric loss tangent (tanδ) has been studied. The nature of variation of the dielectric permittivity with the filler loadings was explained on the basis of interfacial polarization of the filler in the polymer matrix. The effect of filler loading on the real and complex part of the impedance was explained by the relaxation dynamics of the polymer chains in the vicinity of the fillers. The effect of filler and temperature on dielectric loss tangent, dielectric permittivity, AC conductivity, and Nyquist plot was also reported. The bound rubber (BR) value increases with increase in filler loading suggesting the formation of strong interphase, which is correlated with dielectric loss. Thermal activation energy (Ea) was found to be decreasing with the temperature, which follows the Arrhenius relation: τb = τ0 exp(−Ea/KBT) where τb is the relaxation time for the bulk material. From the plot of lnτb versus inverse of absolute temperature (1/T), the activation energies (Ea) were found to be 0.37 and 0.44eV, respectively. The percolation threshold was observed with 40 phr carbon black loading. POLYM. COMPOS., 37:342–352, 2016. © 2014 Society of Plastics Engineers  相似文献   

13.
Dynamic mechanical properties determine the potential end use of a newly developed extruded nylon–wood composite in under‐the‐hood automobile applications. In this article, the dynamic mechanical properties of extruded nylon–wood composites were characterized using a dynamic mechanical thermal analyzer (DMTA) to determine storage modulus, glass transition temperature (Tg), physical aging effects, long‐term performance prediction, and comparisons to similar products. The storage modulus of the nylon–wood composite was found to be more temperature stable than pure nylon 66. The Tg range of the nylon–wood composite was found to be between 23 and 56°C, based on the decrease in storage modulus. A master curve was constructed based on the creep curves at various temperatures from 30 to 80°C. The results show that the relationship between shift factors and temperature follows Arrhenius behavior. Nylon–wood composites have good temperature‐dependent properties. Wood fillers reduced the physical aging effects on nylon in the wood composites. The comparison of the nylon–wood composite with other similar products shows that nylon–wood composites are a promising low cost material for industrial applications. POLYM. COMPOS., 2008. © 2008 Society of Plastics Engineers  相似文献   

14.
Dielectric response of conducting carbon‐black‐filled ethylene–octene copolymer microcellular foams has been investigated with variation of blowing agent and filler loading in the frequency range of 100 Hz to 5 MHz and temperature range from 30 to 100°C. With increase in blowing agent loading, the dielectric permittivity increases for both unfilled as well as carbon‐black‐filled microcellular foams. The experimental complex impedance plots were compared with model‐fitted plots obtained by taking an equivalent circuit of (CQR) (CR).The values of Rb (bulk resistance), Rgb (grain boundary resistance), bulk capacitance (Cb), and grain boundary capacitance (Cgb) at different temperatures were calculated and compared with experimental values. The relaxation time due to bulk effect (τb) has been calculated from relaxation frequency (fr). The dc conductivity (σdc) decreases with rise in temperature indicating the existence of positive temperature coefficient of resistance in the material. The activation energy (Ea) calculated from the relaxation time due to bulk effect (τb) was found to be 0.446 eV, whereas it was 0.363 eV from the dc conductivity plot in the temperature range of 30–100°C. POLYM. COMPOS., 37:3398–3410, 2016. © 2015 Society of Plastics Engineers  相似文献   

15.
The complex shear moduli of the segmented polyurethane Estane 5703p, Livermore explosive (LX)‐14, and plastic bonded explosive (PBX)‐9501, which use this polymer as a binder, have been investigated. Segmented polyurethanes, such as Estane 5703, contain microphase‐separated hard segments in a rubbery matrix of soft segments. LX‐14 is composed of 95.5% 1,3,5,7‐tetranitroazacyclooctane (HMX) explosive with 4.5% Estane 5703 binder. PBX‐9501 is composed of 94.9% HMX, 2.5% Estane 5703p binder, 2.5% nitroplasticizer (NP), and about 0.1% antioxidant Irganox 1010. In the temperature range from ?150 to 120°C, two relaxations were observed as peaks in the loss modulus and tangent delta in Estane 5703p and LX‐14. A third relaxation was found in PBX‐9501. The low temperature relaxation associated with vitrification of the poly(ester urethane) soft segment occurred in the shear loss modulus (G″) at ?29 and ?26°C in Estane and LX‐14, respectively, at 1 Hz. In PBX‐9501 the Estane soft segment glass transition peak, Tg(SS), in the loss modulus occurred at ?40 ± 3°C at 1 Hz. The reduction in soft segment glass transition in PBX‐9501 is clear evidence of plasticization of the soft segment by NP. The apparent activation energy of the maximum in the loss modulus for LX‐14 and PBX‐9501 over the frequency range from 0.1 to 10 Hz was 230 kJ/mole (55 kcal/mole). The hard segment glass transition, Tg(HS), was observed as a peak in the loss modulus at about 70°C. In LX‐14 the transition was observed at lower temperatures (56–58°C at 1 Hz) depending on thermal history. There was a low temperature shoulder on the Tg(HS) of Estane 5703 associated with soft segment crystallinity. Modulated differential scanning calorimetry (MDSC) was used to verify the Tg(HS) in Estane and 50/50 mixtures of Estane with NP. In PBX‐9501 the hard segment glass transition occurred between 65 and 72°C. The presence of NP in PBX‐9501 gave rise to a new transition, Teu(NP), between 8 and 15°C. This peak is believed to be associated with the eutectic melting of the plasticizer. Returns of fielded PBX‐9501 that were 6 and 11 years old were also measured. Small variations in Tg(SS) and the rubber plateau modulus were observed in these aged samples, consistent with migration of plasticizer and/or very low levels of chain scission. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 1009–1024, 2002  相似文献   

16.
This paper presents an inverse method for retrieving (i) the true thermal conductivity, and (ii) the two‐band absorption coefficient of soda‐lime silicate glassmelts between 1100°C and 1550°C from measured steady‐state temperature profiles. This was achieved by combining (i) a forward method solving combined conductive and radiative heat transfer accounting for temperature‐dependent thermal conductivity and spectral absorption coefficient and (ii) an inverse method based on genetic algorithm (GA) optimization. Four glassmelt compositions from ultraclear to gray glasses with iron content ranging from 0.008 to 1.1 wt% were investigated. First, it was established that the steady‐state temperature in glassmelt can be predicted accurately by averaging the spectral absorption coefficient over two bands from 0 to 2.8 μm and 2.8 to 5.0 μm. The inverse method showed that the true thermal conductivity was independent of the iron content and given by kc(T) = 1.31 + 5.90 × 10?4T, where T is given in °C. In addition, the band absorption coefficient between 0 and 2.8 μm strongly increased with increasing iron content, while the band absorption coefficient between 2.8–5.0 μm was independent of iron content.  相似文献   

17.
Dynamic mechanical analysis and dielectric relaxation spectra of exfoliated nano graphite reinforced flouroelastomer composites were used to study their relaxation behavior as a function of temperature (−80°C to +40°C) and frequency (0.01 to 105 Hz). The effect of filler loadings on glass transition temperature was marginal for all the composites and Tg value was in the narrow range of 7.8–8.4°C, which has been explained on the basis of relaxation dynamics of polymer chains in the vicinity of fillers. Strain‐dependent dynamical parameters were evaluated at dynamic strain amplitudes of 0.01–10%. The nonlinearity in storage modulus has been explained on the concept of filler‐polymer interaction and filler aggregation of the nano graphite platelets. The variation in real and complex part of impedance with frequency has been studied as a function of filler. The percolation of the nano graphite as studied by conductivity measurements is also reported. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers.  相似文献   

18.
Melting gels are hybrid gels that have the ability to soften and flow at around 100°C for some combinations of mono‐ and di‐substituted alkoxysiloxanes, where substitutions are either all aromatic or all aliphatic. In this study, melting gels were prepared using phenyltriethoxysilane (PhTES) and dimethyldiethoxysilane (DMDES), meaning both an aromatic and aliphatic substitution. Differential scanning calorimetry was performed to identify glass‐transition temperatures, and thermal gravimetric analysis coupled with differential thermal analysis (TGA‐DTA) was performed to measure weight loss. The glass‐transition temperatures (Tg) ranged from ?61°C to +5.6°C, which are between the values in the methyl only system, where all Tg values are less than 0°C, and those values in the phenyl only system, where Tg values are greater than 0°C. The Tg decreased with an increase in the DMDES fraction. Below 450°C, the gels lost little weight, but around 600°C there was a drop in weight. This temperature is lower than the temperature for gels prepared with only aromatic substitutions, but higher than that for gels prepared with only aliphatic substitutions. Final heat treatment was carried out at 150°C for the gel with 80%PhTES‐20%DMDES (in mol%), and the consolidation temperature increased with increasing DMDES content to 205°C for the gel with 50%PhTES‐50%DMDES. After this heat treatment, the melting gels no longer soften.  相似文献   

19.
The cationic copolymerization of regular soybean oil, low‐saturation soybean oil (LoSatSoy oil), or conjugated LoSatSoy oil with styrene and divinylbenzene initiated by boron trifluoride diethyl etherate (BF3·OEt2) or related modified initiators provides viable polymers ranging from soft rubbers to hard, tough, or brittle plastics. The gelation time of the reaction varies from 1 × 102 to 2 × 105 s at room temperature. The yields of bulk polymers are essentially quantitative. The amount of crosslinked polymer remaining after Soxhlet extraction ranges from 80 to 92%, depending on the stoichiometry and the type of oil used. Proton nuclear magnetic resonance spectroscopy and Soxhlet extraction data indicate that the structure of the resulting bulk polymer is a crosslinked polymer network interpenetrated with some linear or less‐crosslinked triglyceride oil–styrene–divinylbenzene copolymers, a small amount of low molecular weight free oil, and minor amounts of initiator fragments. The bulk polymers possess glass‐transition temperatures ranging from approximately 0 to 105°C, which are comparable to those of commercially available rubbery materials and conventional plastics. Thermogravimetric analysis (TGA) indicates that these copolymers are thermally stable under 200°C, with temperatures at 10% weight loss in air (T10) ranging from 312 to 434°C, and temperatures at 50% weight loss in air (T50) ranging from 445 to 480°C. Of the various polymeric materials, the conjugated LoSatSoy oil polymers have the highest glass‐transition temperatures (Tg) and thermal stabilities (T10). The preceding properties that suggest that these soybean oil polymers may prove useful where petroleum‐based polymeric materials have found widespread utility. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 658–670, 2001  相似文献   

20.
The xBi(Zn2/3Nb1/3)O3–(1?x)(K0.5Na0.5)NbO3 (abbreviated as xBZN–(1?x)KNN) ceramics have been synthesized using the conventional solid‐state sintering method. The phase structure, dielectric properties and “relaxorlike” behavior of the ceramics were investigated. The 0.03BZN–0.97KNN ceramics show a broad and stable permittivity maximum near 2000 and lower dielectric loss (≤5%) at a broad temperature usage range (100°C–400°C) and the capacitance variation (ΔC/C150°C) is maintained smaller than ±15%. The 0.03BZN–0.97KNN ceramics only possess the diffuse phase transition and no frequency dispersion of dielectric permittivity, which indicates that 0.03BZN–0.97KNN ceramics is a high temperature “relaxorlike” ferroelectric ceramics. These results indicate that 0.03BZN–0.97KNN ceramics are excellent promising candidates for preparing high‐temperature multilayer ceramics capacitors.  相似文献   

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