烧结工艺对Ca3Co4O9基热电氧化物电性能的影响

采用溶胶-凝胶化学法合成了Ca3Co4O9热电氧化物粉末,分别采用陶瓷烧结工艺方法和放电等离子烧结(Spark Plasma Sintering,SPS)的方法制备了Ca3Co4O9热电氧化物块体材料.利用X射线衍射XRD、扫描电子显微镜SEM和电输运参数测试仪分析了所得样品的物相、微观组织结构、晶粒取向度和电输运性能.结果表明,不同制备方法均可得到纯相的Ca3Co4O9热电氧化物块体材料;通过陶瓷烧结工艺方法制备的Ca3Co4O9热电氧化物块体晶粒取向度较低,但随着成型压力的增加而提高;SPS烧结的方法制备的Ca3Co4O9热电氧化物块体晶粒取向度最高;试样电性能随着晶粒取向度的提高逐渐提高,其中SPS烧结方法制备的块体材料电性能最高,在测试温度最高点700℃时功率因子达3.85 μWmK-2,远高于普通烧结试样.     

多晶YAG陶瓷的制备及力学性能

本实验采用共沉淀方法制备YAG微粉 ,Al和Y元素分布均匀 ,在 90 0℃煅烧 2h即可全部转变为YAG粉体 ,无过渡相 .15 0 0℃热压 1h可获得致密烧结体 ,其抗弯强度为 2 45MPa ,断裂韧性为 2 .0MPa·m1 /2 ,晶粒大小为 3～ 6μm ;14 0 0℃放电等离子烧结 5min可获得相对密度为 93 %的烧结体 ,其抗弯强度为 3 4 8MPa,断裂韧性为 2 .1MPa·m1 /2 ,晶粒大小为 1～ 2 μm .     

不同粉体制备工艺对Ca3Co4O9陶瓷性能的影响

采用溶胶凝胶法和化学共沉淀法制备了Ca3Co4O9粉体,并烧结为纯相Ca3Co4O9陶瓷。利用XRD、SEM等方法对陶瓷样品的物相以及断面形貌进行了表征,利用四探针法测量了Ca3Co4O9陶瓷的电导率。试验结果表明化学共沉淀法与溶胶凝胶法粉体相比,制得的Ca3Co4O9陶瓷不仅具有更低的气孔率、线收缩率,而且具有更高的电导率,也是一种制备高性能热电材料粉体的有效方法。     

溶胶-凝胶法制备巨介电常数材料CaCu3Ti4O12

通过溶胶-凝胶法制备CaCu3Ti4O12干凝胶,再经700～900℃,6～10h预烧和950～1 100℃,16～20h烧结,成功制备了CaCu3Ti4O12粉体和CaCu3Ti4O12巨介电常数陶瓷材料.用X射线衍射、扫描电镜分别确定了样品的结晶性能和形貌.用阻抗分析仪在10～106Hz范围内测试了陶瓷样品的介电性能.结果表明:粉体的结晶性能与煅烧温度有关,陶瓷介电性能与其晶粒大小有关.相对于传统固相反应合成法制备的粉体和陶瓷,粉体的预烧和陶瓷的烧结温度都有明显降低,烧成温度至少降低100℃.在800℃预烧的CaCu3Ti4O12粉体并在1 100℃温度下烧结制备的陶瓷,其介电常数可达194753.     

微波加热法制备Ca3-xLaxCo4O9热电材料

采用微波加热法合成了稀土La掺杂的Ca3-xLaxCo4O9材料的前驱粉末,进一步制备了热电材料烧结体.通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)等对材料的微观结构进行了研究,通过电导率的测量、Seebeck系数以及热导率的计算研究了材料的热电性能.实验结果表明,微波加热法可以在较短的时间内制得Ca3-xLaxCo4O9粉体,微波烧结方法时间短,效率高,并且晶粒生长完善且晶粒细小.Ca3-xLCo4O9热电材料的微观结构为片状结构,晶粒生长完整.     

放电等离子烧结钛酸钡陶瓷的碳污染及脱碳工艺研究

为了研究放电等离子烧结钛酸钡陶瓷过程中的碳污染及脱碳工艺,以钛酸钡粉体为原料,用石墨模具,以碳纸为脱模包覆材料,在1150℃、50MPa条件下进行放电等离子烧结。用XRD对脱碳前后烧结体进行物相分析,用能谱仪对不同脱碳时间下的烧结体的碳元素的分布进行线分析,用扫描电镜观察脱碳时间对组织的影响。结果表明：石墨模具会污染钛酸钡烧结体,碳元素沿烧结体半径方向呈梯度分布；脱碳温度为800℃时,保温2小时能够完全除去烧结体内的碳污染,并得到致密、组织均匀的钛酸钡陶瓷。     

AlN-Re2O3液相烧结碳化硅

采用非氧化物AlN和Re2O3作为复合烧结助剂(Re2O3-La2O3与Y2O3)进行碳化硅液相烧结得到了致密的烧结体.烧结助剂占原料粉体总质量的20%,其中:AIN与(La0.5Y0.5)2O3的摩尔比为2:1,在30MPa压力下,1850℃保温0.5h热压烧结的碳化硅陶瓷,抗弯强度>800MPa,断裂韧性>8MPa·m1/2,明显高于同组分1 950℃无压烧结0.5h的碳化硅陶瓷的抗弯强度(433.7MPa)和断裂韧性(4.8MPam·m1/2.热压烧结的陶瓷晶粒呈单向生长,断裂模式为沿晶断裂.同组分无压烧结碳化硅陶瓷的显微结构可以观察到核壳结构.     

3Y-ZrO2/Al2O3复合粉体制备工艺研究

以Al(NO3)3·9H2O和ZrOCl2·8H2O为主要原料,采用醇-水溶液加热结合共沉淀法制备出前驱体。利用DTA-TG和X射线衍射(XRD)分析研究了前驱体的煅烧过程。结果显示,275℃时前驱体已完全分解为非晶态氧化物,800℃时t-ZrO2开始结晶,至1150℃时出现α-A12O3晶体,获得3Y-ZrO2/A12O3复合粉体。该复合粉体在1400℃下常压烧结,可得到相对密度达90.4%的ZTA陶瓷。     

SrBi4Ti4O15铁电陶瓷的制备工艺研究

研究了固相反应合成SrBi4Ti4O15粉末的反应过程及不同预烧温度对SrBi4Ti4O15铁电陶瓷物相结构的影响。对不同工艺条件对SrBi4Ti4O15铁电陶瓷相对密度的影响进行了讨论，确定最佳工艺条件，预烧温度900℃，烧结温度为1100℃(Al2O3埋烧)。     

高密度LiNi_(0.8)Co_(0.2)O_2的合成

以二次干燥化学共沉淀法制得高密度前驱体Ni0.8Co0.2(OH)2,再与LiNO3混合,经600℃恒温6 h,800℃恒温24 h两个恒温阶段烧结,得到高密度LiNi0.8Co0.2O2,探讨了锂源、镍源、Li/(Ni+Co)摩尔比、合成温度等因素对产品的影响,优化了LiNi0.8Co0.2O2的合成工艺。所得非球形LiNi0.8Co0.2O2粉末振实密度高达3.15 g/cm3,大幅度地提高正极材料的体积比能量。X射线衍射分析表明,合成的LiNi0.8Co0.2O2具有规整的层状NaFeO2结构,充放电测试表明,材料具有良好的电化学性能。     

Ca3Co4O9陶瓷的制备与表征

本实验采用溶胶-凝胶法制备了Ca3Co4O9陶瓷,寻求了其合适的制备工艺,并对陶瓷的显微结构、物相组成、元素组成等进行了表征测试.实验结果表明:煅烧温度为800～900 ℃时均能得到纯相Ca3Co4O9;Ca3Co4O9为取向无规则层片状组织,颗粒尺寸均匀,为2 μm左右;样品的致密度不高,气孔率相对较大.     

Photoluminescence Properties of Nanocrystalline ZnO Ceramics Prepared by Pressureless Sintering and Spark Plasma Sintering

Nanocrystalline ZnO ceramics with grain sizes of ∼100 nm were prepared by pressureless sintering at 800°C for 2 h and spark plasma sintering (SPS) at 550°C for 2 min, respectively. Excellent green emission properties were obtained in the ZnO ceramic prepared by the SPS process and in the pressureless-sintered ZnO ceramic prepared at 1000°C for 2 h, which are attributed to the vacuum ambience of the SPS process and the sublimeness of the interstitial Zn at >900°C in air, respectively.     

Preparation of Ca3Co4O9 and Improvement of its Thermoelectric Properties by Spark Plasma Sintering

The precursor powders of Ca₃Co₄O₉ were synthesized by a sol–gel method. The results of X-ray diffraction and thermogravimetric and differential thermal analyses patterns indicate that pure Ca₃Co₄O₉ powders could be obtained by calcining the precursor at 800°C for 2 h. High dense Ca₃Co₄O₉ ceramic samples (∼99% of theoretical density) were prepared by the spark plasma sintering (SPS) method. Compared with the conventional sintering (CS), the SPS samples exhibit much higher electrical conductivity and power factor which are respectively about 118 S/cm and 3.51 × 10⁻⁴ W·(m·K²)⁻¹. The SPS method is greatly effective for improving the thermoelectric properties of Ca₃Co₄O₉ oxide ceramics.     

Microstructure and flexural strength of hafnium diboride via flash and conventional spark plasma sintering

Microstructure evolution in bulk hafnium diboride ceramics prepared by spark plasma sintering in flash regime was compared with conventional spark plasma sintering. The conventional and flash spark plasma sintering resulted in ceramics with a high relative density exceeding 96% of their theoretical density. A remarkably fine grain size distribution was noticed for the specimen prepared in the flash regime. This atypical microstructure evolution provides a possible insight into the mechanism of flash sintering for conductive bulks. The room temperature flexural strength of the hafnium diboride processed by flash SPS was 650 MPa which is 140 MPa higher than the sample produced by conventional SPS.     

红色荧光粉Ca2La8Si6O26:Eu的制备和性能

采用高温固相法合成新型CaeLasSi6O26:Eu红色荧光粉,利用X射线衍射、扫描电镜及荧光光谱对其进行了表征.结果表明:合成的Ca2LasSi6O26:Eu属于六角晶系,可被近紫外光(394 nm)和蓝光(464 nm)有效激发,发射峰值位于614 nm(对应于Eu3+的5D0→7F2跃迁),激发波长与目前广泛使用...     

不同烧结气氛下制备的AlN陶瓷结构和电性能的差异

以AlN粉末为原料、Y2O3粉末为烧结助剂,分别在氮气气氛下和真空气氛下,采用放电等离子烧结方法在1700℃、25MPa条件下保温10min制备AIN陶瓷。X-射线衍射、扫描电镜和X-射线光电子能谱分析表明：不同烧结气氛下制备的AlN陶瓷的结构和体积电阻率各有不同。真空气氛AlN陶瓷与氮气气氛AlN陶瓷相比较,除舍有主晶相AlN和第二相Y3Al5O12外,还含有微量Al2Y相。正是由于微量Al2Y相的存在,使得真空气氛下得到的AlN陶瓷比氮气气氛下得到的A1N陶瓷的体积电阻率低约2个数量级。     

Effects of phase constitution and microstructure on energy storage properties of barium strontium titanate ceramics

Barium strontium titanate (Ba_0.3Sr_0.7TiO₃, BST) ceramics have been prepared by conventional sintering (CS) and spark plasma sintering (SPS). The effects of phase constitution and microstructure on dielectric properties, electrical breakdown process and energy storage properties of the BST ceramics were investigated. The X-ray diffraction analysis and dielectric properties measurements showed that the cubic and tetragonal phase coexisted in the SPS sample while the CS sample contained only tetragonal phase. Much smaller grain size, lower porosity, fewer defects and dislocation were observed in SPS samples, which greatly improved the electrical breakdown strength of the Ba_0.3Sr_0.7TiO₃ ceramics. The enhanced breakdown strength of the SPS samples resulted in an improved maximum electrical energy storage density of 1.13 J/cm³ which was twice as large as that of the CS sample (0.57 J/cm³). Meanwhile, the energy storage efficiency was improved from 69.3% to 86.8% by using spark plasma sintering.     

硼硅酸盐玻璃成分对硫酸钡热稳定性的影响

研究了硼硅酸盐玻璃主要成分(SiO2、Na2O、B2O3)对硫酸钡(BaSO4)热稳定性的影响,分析BaSO4分别与SiO2、Na2O、B2O3的混合物在不同温度(800~1 200℃)煅烧后的物相组成、显微结构、硫含量和拉曼光谱。结果表明:当BaSO4:SiO2摩尔比为7.5:92.5 (样品A)时,在温度低于1 200℃煅烧后其物相均为BaSO4和SiO2,温度达到1 200℃时出现了少量硅钡石(BaSi2O5)相;当BaSO4:SiO2:Na2O为7:86:7 (样品B)时,在800℃煅烧后即出现了少量BaSi2O5相,当温度达到1200℃时样品主要物相为BaSi2O5和方石英,硫含量明显减少;当BaSO4:SiO2:Na2O:B2O3为5.5:67.5:6.5:21.5 (样品C)时,在800~1 200℃均为BaSO4和SiO2,在1 200℃保温2h后,BaSO4和SiO2的衍射峰基本消失。低熔点的Na2O和B2O3的引入促进了BaSO4的分解,在1 200℃煅烧后,样品A、B、C中SO4四面体的拉曼特征峰依次减弱。     

A new process for lamellar texturing of thermoelectric Ca3Co4O9 oxides by spark plasma sintering

Processing of textured Ca₃Co₄O₉ (Ca349) thermoelectric ceramics with a good platelet orientation by spark plasma sintering (SPS) consolidation is reported. Two configurations wherein: (i) the oxide powder, being directly introduced into the graphite mould and (ii) placing a compact pellet prepared from the oxide powder in the centre of the mould have been investigated. The free deformation configuration route is found to improve the microstructure and transport properties of Ca₃Co₄O₉ TE oxides. The material prepared exhibited a better performance than the sample obtained by conventional SPS way.