Spectroscopic studies and Rietveld refinement of strontium-britholites

Strontium-britholites whose chemical formula was Sr10-xLax（PO4）6-x（SiO4）xF2, where x=0, 1, 2, and 4 were prepared by solid state reaction. The structural refinement carried out using the Rietveld method indicated that La^3＋ ions were located into the two sites with a strong preference for metal （2） sites especially for low contents. A progressive shift of the F position along the c-axis outside the centre of the triangle formed by metal （2）-atoms was observed with the increase of x. The infrared and Raman spectra exhibited the characteristic vibration modes of PO4 and SiO4groups confirming the incorporation of this last group into the apatite structure. The 295i MAS-NMR spectra exhibited one resonance peak confirming the data obtained by X-ray diffraction, indicating that P and Si were located in the same crystallographic site.     

Thermodynamical Evaluation on Magnetocaloric Effect of Magnetic Refrigerating Materials Near Room Temperature

The relationship between isothermal magnetic entropy change △S and adiabatic temperature change △Tad was deduced according to the principles of thermodynamics. The MCE and the engineering application were discussed for Gd and several new kinds of magnetic refrigerating materials near room temperature, Gd5Si2Ge2, MnFeP0.45As0.55 and LaFe11.2Co0.7Si1.1. Isothermal entropy change is proportional to adiabatic temperature change with a factor of T/C (T is temperature, C is heat capacity). When the comparison of magnetacoloric effect is made for two different materials, we should consider isothermal entropy change as well as adiabatic temperature change.     

Phase formation with NaZn13 structure in metamagnetic La（Fe1-xCox）11.9Si1.1 compounds

The effects of different annealing conditions on the phase formation with NaZn13 structure were investigated in La（Fe1-xCox）11.9Si1.1 （x=0.068） compounds. It was found that the 1：13 phase was not formed directly from the melt upon cooling but via a peritectic reaction between the pro-peritectic γ-Fe and the La-rich phase. Annealing temperature was very important for the formation of 1：13 phase. Ice water was confirmed to be a preferable quenching medium. La（Fe1-xCox）11.9Si1.1 （x=0.068） compounds with almost single 1：13 phase were obtained at 1473 K after 15 d.     

Research Advance on Magnetocaloric Effect of La-Fe-M（AI，Si） Compounds

Recent research progress on magnetocaloric effect of La-Fe-M (M=Al,Si) compounds was presented. La-Fe-M(M=A1,Si) compounds of high Fe content are excellent soft magnetic materials with NaZn13 structure. The Curie temperature of the compounds can be increased by substituting small amount of Co for Si, Al. The La(Fe1_yCoy)xSi13-x compoundswith an appropriate ratio of Co and Si can produce giant magnetocaloric effect comparable to that for Gd5Si2Ge2 at room temperature. The La(FexSi1-x)13 doped with H can also produce giant magnetocaloric effect at room temperature,which is much greater than that for Gd. For La(FexSi1-x)13 compounds with low Si or high Si contents. The nature of phase transition near Curie temperature induced by temperature and magnetic field was described in detail.     

Effect of praseodymium and cobalt substitution on magnetic properties and structures in La(Fe_(1–x)Si_x)_(13) compounds

Magnetic properties and structures in La1-zPrz(Fe0.895–xCoxSi0.105)13 (x=0.07, 0.08; z=0, 0.2, 0.4) compounds were investigated. When Pr and Co substituted for La and Fe, the Curie temperature of the compounds was adjusted to around room temperature. The magnetic phase transition was driven from first-order to second-order due to Co substitution. As a second-order phase transition material, the MCE of La0.6Pr0.4(Fe0.825Co0.07Si0.105)13, whose relative cooling power was 175 J/kg under a field change of 2 T, ...     

Phase,microstructure, and magnetocaloric effect of the large disc LaFe11.6Si1.4 alloy

The large disc LaFe11.6Si1.4 alloy, which was prepared by medium-frequency induction furnace, was annealed at 1503 K for different time. The main phases were 1:13 phase in the edge parts of the large discs alloy; the impurity phases included α-Fe phase, LaFeSi phase, and even very small amount of La5Si3 phase. The amounts of impurity phases reduced with increasing in annealing time. The magnetic properties in the edge parts of the large discs LaFe11.6Si1.4 alloy were investigated. The magnetic susceptibility had an abrupt change at Curie temperature(TC) as the magnetization in M-T curves. The alloys had almost the same TC(191 K), the magnetocaloric effect(MCE) and relative cooling power(RCP) increased with increasing in annealing time. In addition, for the same alloy, the magnetic hysteresis decreased with the increase in temperature.     

不同工艺对LaFe11.9-xCoxSi1.1B0.25(x=0.7,0.8)合金的磁热效应的影响

从室温磁制冷商品化角度出发,用工业纯原料,对用不同工艺(甩带、铸锭)制作的LaFe11.9-xCoxSi1.1B0.25(x=0.7,0.8)合金的磁热效应作了研究.研究结果表明,铸锭样品的磁热效应优于甩带样品,在1.5T磁场下,铸锭LaFe11.2Co0.7Si1.1B0.25样品的温变最大值达到2.6K,对应的温度在-6℃左右.随着Co的加入,居里温度升高,但磁热效应有所降低.     

Influence of gadolinium on microstructure and magnetic properties of sintered NdGdFeB magnets

The effect of Gd content on microstructure and magnetic properties of sintered Nd33.03-xGdxFe65.65B1.32 (x=0-2) was studied in this paper to improve the thermal stability of NdFeB and to reduce the raw material cost. The results showed that better magnet performance could be obtained by adding Gd (0-1.5 wt.%) with partial substitution of Nd in Nd33.03-xGdxFe65.65B1.32. It was also found that the Nd33.03-xGdxFe65.65B1.32 magnets showed the best performance when Gd addition increased to 1.0 wt.%. The temperature coefficient Br (α) could be improved from -0.15%/oC to -0.063%/oC (maximum work temperature 120 oC) and the Curie temperature could be improved from 315 oC to 323 oC because the Gd2Fe14B had positive temperature coefficient Br (α) and higher Curie temperature than that of Nd2Fe14B. The coercivity could be improved from 10.2 to 11.48 kOe and the microstructure was close to ideal microstructure. The magnetic performance decreased sharply by adding Gd (above 2 wt.%) with partial substitution of Nd in Nd33.03-xGdxFe65.65B1.32 because the Gd element concen-trated in the grain boundaries.     

Investigation of the crystal structure and magnetic properties of Nd_（3-x）GdxCo_（11）B_4 borides

Polycrystalline samples of pseudo-ternary intermetallic Nd3-xGdxCo11B4 (x=0,1,2,3) borides prepared by standard arc-melting were characterized by X-ray powder diffraction (XRPD),magnetization and differential scanning calorimetry (DSC) measurements. The X-ray diffraction patterns indicated the hexagonal Ce3Co11B4-type structure with P6/mmm space group for each composition. The substitution of Gd for Nd led to a decrease of the unit-cell parameters a and the unit-cell volume V,while the unit-cell parameter c increased linearly. Magnetic measurements indicated that all samples were ordered magnetically below the Curie temperature. The Curie temperatures increased as Nd was substituted by Gd. The saturation magnetization at 4 K decreased upon the Gd substitution up to x=1,and then increased.     

Synthesis and photoluminescence properties of Ca3R2-xWO9:xEu3+(R=Y,Gd) phosphors

Ca3R2–xWO9:xEu3+(R=Y, Gd) red-emitting phosphors were prepared by solid state reactions. These samples were characterized by differential scanning calorimetry and thermogravimetry analysis(DSC-TGA), X-ray diffraction(XRD), Fourier transform infrared spectroscopy(FTIR), photoluminescence(PL) and field emission scanning electron microscopy(FE-SEM) analyses. The optimum sintering temperature for these phosphors was 1100 oC, and the optimum sintering time was 2 h. The optimum doped concentration of Eu3+3+ in Ca3Y2–xWO9:xEu and Ca3Gd2–xWO9:xEu3+ were x=1.5 and x=1.1, respectively. These phosphors could be excited by near-UV light of 394 nm and blue light of 465 nm, and showed strong red emission line at 612 nm(5D0→7F2), which indicated that Ca3R2–xWO9:xEu3+(R=Y, Gd) were promising red candidates for white LED.     

Synthesis and characterization of calcium and manganese-doped rare earth oxide La_(1-x)Ca_xFe_(0.9)Mn_(0.1)O_(3-δ) for cathode material in IT-SOFC

In order to develop novel cathode materials with high performance for intermediate temperature SOFC(IT-SOFC),Ca and Mn doped rare earth oxides La1-xCaxFe0.9Mn0.1O3-δ(x=0.1,0.3 and 0.5,denoted as LCFM9191,LCFM7391 and LCFM5591) were synthesized by solid state reaction(SSR) method.The formation process,phase structure and microstructure of the synthesized samples were characterized using thermogravimetry/differential scanning calorimetry(TG/DSC),X-ray diffraction(XRD) and scanning electron microscopy(SEM).The thermal expansion coefficients(TEC) of the samples were analyzed at 100-900 oC by thermal dilatometry.The electrical conductivities of the samples were measured with direct current(DC) four-terminal method from 300 to 850 oC.The results indicated that the samples(x=0.1 and 0.3) exhibited a single phase with orthorhombic and cubic perovskite structure,respectively after being sintered at 1200 oC for 3 h.The electrical conductivity of the samples increased with temperature up to a maximum value,and then decreased.The small polaron hopping was regarded as the conducting mechanism for synthesized samples at T≤600 oC.The negative temperature dependence occurring at higher temperature was due to the creation of oxygen vacancies for charge balance.LCFM7391 had higher mixed conductivity(>100 S/cm) at intermediate temperature and could meet the demand of cathode material for IT-SOFC.In addition,the average TECs of LCFM9191 and LCFM7391 were 11.9×10-6 and 13.1×10-6 K-1,respectively,which had good thermal match to the common electrolytes.     

Nanocrystalline Gd_(1–x)Ca_xFeO_3 sensors for detection of methanol gas

The sol-gel method was used to prepare the nanocrystalline Gd_(1–x)Ca_xFeO_3 (x=0–0.4) powders. The XRD results showed that all the Gd_(1–x)Ca_xFeO_3 (x=0–0.4) compounds crystallized as perovskite phase with orthorhombic structure. The doping of Ca in GdFeO_3 not only reduced the resistance, but also enhanced the response to methanol. The Gd_(0.9)Ca_(0.1)FeO_3 showed the best response to methanol among Gd_(1–x)Ca_xFeO_3 sensors. Besides, it showed good selectivity to methanol among methanol, ethanol, CO and formaldehyde gases. The responses at 260 oC for Gd_(0.9)Ca_(0.1)FeO_3-based sensor to 600 ppm methanol, ethanol and CO gases were 117.7, 72.7 and 31.9, respectively. Even at quite low gas concentrations, Gd_(0.9)Ca_(0.1)FeO_3-based sensor had an obvious response. At 260 °C, the response of 1.54 was obtained to be 45 ppm methanol. The experimental results showed that nanocrystalline Gd_(0.9)Ca_(0.1)FeO_3 based sensor can be used to detect methanol gas.     

Sintering behavior and microwave dielectric properties of （1-x）CaTiO_3-xLaAlO_3 ceramics

The sintering behavior,microstructure and microwave dielectric properties of (1–x)CaTiO3–xLaAlO3 (x=0.1,0.3,0.5,0.7,0.9,respectively) ceramics were investigated systematically by thermogravimetry-differential thermal analysis (TG-DSC),X-ray diffraction (XRD),scanning electron microscopy (SEM) and a network analyzer.The result showed that forming temperature of the perovskite type crystal increased with increasing of x value.0.9CaTiO3-0.1LaAlO3 ceramics were sintered well from 1 400 to 1 550 oC,its bulk density increased with sintering temperature,and microwave dielectric properties of the ceramics at 1 400 oC was shown as follows: relative dielectric constant εr= 45.1,Q×f= 46 087 GHz and τf=–14.1×10–6/oC,respectively.But 0.7CaTiO3-0.3LaAlO3 ceramics were sintered well only when sintering temperature rose to 1 500 oC.(1–x)CaTiO3–xLaAlO3 (x=0.5,0.7 and 0.9,respectively) were not sintered well up to 1 550 oC and the sintered samples exhibited porous characteristic and with low bulk density.     

Microwave assisted synthesis,sinterability and properties of Ca-Zn co-doped LaCrO_3 as interconnect material for IT-SOFCs

The interconnect materials La0.7Ca0.3Cr1-xZnxO3-δ(x=0,0.01,0.03,0.05,0.07) were prepared by a microwave assisted sol-gel auto-ignition process.The crystalline structures of the samples were characterized by X-ray diffraction(XRD) and the lattice parameters were evaluated with Rietveld method.For Ca-Zn co-doped LaCrO3 with x=0.03,the sintering activity was improved,and the relative density came up to 96.5% for the sample sintered at 1300 oC for 10 h.The electrical conductivity of the samples was increased from 21.1 S/cm to the maximum of 70.9 S/cm at 650 oC in air,with the x content increasing from 0.01 to 0.03.However,with x further increasing,the electrical conductivity was decreased.The average thermal expansion coefficient(TEC) of the samples at RT-1000 oC in air was ca.10.0×10-6 K-1.All data indicated that the La0.7Ca0.3Cr1-xZnxO3-δ series ceramics would be potential candidate to be used as an interconnect materials for IT-SOFCs.     

Crystal structure and magnetic behavior of the La0.1Bi0.9FeO3 compound

The nano-crystalline La_(0.1)Bi_(0.9)FeO_3 compound was successfully synthesized by starch-based combustion method. The crystal structure and magnetic behavior were studied by temperature-dependent X-ray diffraction(XRD), scanning electron microscopy(SEM), differential scanning calorimetry(DSC) and magnetic measurements. The La_(0.1)Bi_(0.9)FeO_3 compounds crystallized in a rhombohedrally distorted perovskite structure with space group R3 c. The substitution of La for Bi reduced the rhombohedral distortion. The structural phase transitions in La_(0.1)Bi_(0.9)FeO_3 driven by temperature showed that the extraordinary two-phase coexistence state of BiF eO 3 and LaF eO 3 was observed in a narrow temperature range of 630–700 oC. The magnetization of the La_(0.1)Bi_(0.9)FeO_3 sample was improved by heat treatment in the temperature range. When the heat treatment temperatures rose from 25 to 600 oC, the remanence(Mr) and coercivity(Hc) of the La_(0.1)Bi_(0.9)FeO_3 compound almost remained the same, and increased rapidly to 0.134 emu/g and 7.1 KOe on further increasing the heat treatment temperature to 650 oC.     

Influence of partial substitution of cerium for lanthanum on magnetocaloric properties of La_(1–x)Ce_xFe_(11.44)Si_(1.56) and their hydrides

The structure and magnetocaloric properties of La1–xCexFe11.44Si1.56 and their hydrides La1–xCexFe11.44Si1.56Hy（x=0, 0.1, 0.2, 0.3, 0.4） were investigated.The samples crystallized mainly in the cubic Na Zn13-type structure with a small amount of α-Fe phase as impurity.The lattice constants and Curie temperature presented the same change tendency with increasing of Ce content.For the hydrides, the influence of Ce content on lattice constants was weakened and the values of H concentration y were approximate to be 1.56.The La1–xCexFe11.44Si1.56 compounds exhibited large values of isothermal entropy change –ΔSm around the Curie temperature TC under a low magnetic field change of 1.5 T.The value of –ΔSm increased and then decreased with increasing Ce content, reached the maximum, 26.07 J/kg·K for x=0.3.TC increased up to the vicinity of room temperature by hydrogen absorption for the Ce substituted compounds, but TC only slightly decreased with increasing Ce content.The first-order metamagnetic transition was still kept in the hydrides and the maximum values of –ΔSm were lower than those of the La1–xCexFe11.44Si1.56 compounds, but still remained large values, about 10.5 J/kg K under a magnetic field change of 1.5 T.The values of –ΔSm were nearly independent of the Ce content and did not increase with increasing x for the hydrides.The La1–xCexFe11.44Si1.56Hy（x=0–0.4） hydrides exhibited large magnetic entropy changes, small hysteresis loss and effective refrigerant capacity covered the room temperature range from 305 to 317 K.These hydrides are very useful for the magnetic refrigeration applications near room temperature under low magnetic field change.     

Effects of Hot Bending Parameters on Microstructure and Mechanical Properties of Weld Metal for X80 Hot Bends

Mechanical properties of weld metal are the key factors affecting the quality of heavy-wall X80 hot induction bends. The effects of bending parameters on the mechanical properties of weld metal for hot bends were investigated by simulation conducted on a Gleeble 3500 thermal simulator. Continuous cooling transformation （CCT） dia- grams of the weld metal were also constructed. The influences of hot bending parameters （such as reheating temperature, cooling rate, and tempering temperature） on the microstructure and mechanical properties of weld metal were also analyzed. Results show that the strength of all weld metal specimens is higher than the value indicated in the technical specification and increases with the increase of reheating temperature, cooling rate, and tempering tempera ture. The impact toughness is apparently related to the variation of reheating temperature, cooling rate, and tempering temperature.     

Preparation and performance of Pr-doped Ba_(0.5)Sr_(0.5)Co_(0.8)Fe_(0.2)O_(3-δ) cathode for IT-SOFCs

(Ba0.5Sr0.5)1-xPrxCo0.8Fe0.2O3-δ(BSPCFx;x=0.00-0.30) oxides were synthesized by a sol-gel thermolysis process using combination of PVA and urea,and were also investigated as cathode material for intermediate temperature solid oxide fuel cells(IT-SOFCs).X-ray diffraction(XRD) results showed that all the samples formed a single phase cubic pervoskite-type structure after being calcined at 950 oC for 5 h and the lattice constant decreased with the Pr content increasing.The electrical conductivity of Ba0.5Sr0.5Co0.8Fe0.2O3-δ(BSCF) was greatly enhanced by Pr-doping.The thermal expansion coefficient(TEC) of BSPCFx was increased with the content of Pr increasing,and all the thermal expansion curves had an inflection at about 250-400 oC due to the thermal-induced lattice oxygen loss and the reaction of Co and Fe ion.Ac impedance analysis indicated that BSPCFx possessed better electrochemical performance.The polarization resistance of the sample with x=0.2 was only ～0.948 Ω cm2 at 500 oC,significantly lower than that of BSCF(～2.488 Ω cm2).     

Microstructure evolution and corrosion properties of Mg-Dy-Zn alloy during cooling after solution treatment

Microstructure evolution and corrosion properties of Mg-2Dy-0.5Zn(at.%) alloy during cooling after solution treatment were investigated.The microstructure of alloy in the solid solution state(530 oC,12 h) was composed of α-Mg and small amounts of(Mg,Zn)_x Dy phases.During cooling at a cooling rate of 2 oC/min,the 14H-type LPSO phase gradually precipitated in the grain interior and its volume fraction increased with increasing cooling time.The alloy cooled for 20 min exhibited the highest hardness value.In addition,electrochemical and immersion test results indicated that the alloy cooled for 5 min exhibited small corrosion current and low corrosion rate.The good corrosion resistance of alloy was mainly attributed to the continuous distribution of LPSO phase along the grain boundary.     

Crystal structure and hard magnetic properties of TbCu_7-type Sm_(0.98)Fe_(9.02–x)Ga_x nitrides

The compound Sm0.98Fe9.02–xGaxNδ(x=0, 0.25, 0.5, 0.75, 1) were prepared by melt-spun method and subsequent annealing and nitriding. The Rietveld analysis showed that the lattice expansion played an important role in improving the Curie temperature. An obvious development of the Curie temperature was obtained with the increased Ga content from x=0–1(ΔTc=90 oC). The optimum coercivity of nitrides was obtained at x=0.25 with the value Hcj=652 kA/m(8.15 kOe) after annealing, which corresponded to a reasonable distribution of grain sizes of both TbCu7-type SmFe9Nδ and α-Fe. However, an excess of Ga doping might lead to an abnormal growth of α-Fe, which in turn deteriorated the magnetic properties. It was concluded that a moderate Ga content was very effective in raising the coercivity and Curie temperament in the TbCu7-type Sm-Fe-N.