冷冻干燥法制备高气孔率、低介电的Si_3N_4陶瓷

采用冷冻干燥法制备具有低介电、定向双峰孔径分布的多孔Si_3N_4陶瓷,并利用Zeta电位、流变仪研究分散剂种类、含量及pH值对浆料的影响。结果表明:当分散剂为聚丙烯酸铵(NH_4-PAA)且其含量为0.8%(质量分数),浆料pH值在10左右时浆料的分散效果最好。利用压汞仪、XRD、SEM与矢量网络分析仪研究了粘结剂含量与固相含量对多孔陶瓷微观结构与性能的影响。结果表明:随着粘结剂含量与固相含量的增加,陶瓷的气孔率下降,力学性能增强。当固相含量由15%(体积分数)增加至40%(体积分数)时,气孔率由82.9%降低至40.6%,抗弯强度由(1.2±0.2) MPa增加到(94.7±5) MPa,抗压强度由(2.1±0.5) MPa增加到(314±8) MPa,介电常数由1.5增加至3.7(12.4～18 GHz波段内)。通过冷冻干燥法制备的多孔Si_3N_4陶瓷在过滤、催化剂载体、透波材料等领域具有更广阔的应用。     

浆料粘度对纳米羟基磷灰石/聚酰胺66复合支架孔结构与力学性能的影响

浆料粘度是热诱导相分离法制备支架材料的关键因素,采用不同粘度的纳米羟基磷灰石/聚酰胺66(n-HA/PA66)复合浆料制备了相应的n-HA/PA66多孔支架,并对不同粘度浆料制备支架材料的泡孔结构和力学性能等进行了对比研究。结果表明,浆料粘度对n-HA/PA66复合多孔支架的孔径、孔径分布、孔隙率、开孔率、力学强度等性能有显著的影响。随着浆料粘度的增大,制备支架的孔径、孔隙率、开孔率逐渐减小,而力学强度却逐渐增大。当浆料粘度为330Pa.s时,制备出的n-HA/PA66复合多孔支架综合性能最好,其孔径主要分布在200～500μm,平均孔径(324±67.1)μm,孔隙率为(75±1.6)%,开孔率为(59±2.5)%,抗压强度为(2.12±0.90)MPa,能够较好地满足骨组织工程支架材料对孔径、孔隙率和力学性能的要求。     

叔丁醇基凝胶注模工艺制备轻质、高强莫来石多孔陶瓷

以叔丁醇为成型溶剂, 莫来石粉为起始原料, 采用凝胶注模成型方法制备出轻质、高强莫来石多孔陶瓷. 莫来石多孔陶瓷中的孔隙形成于干燥过程中叔丁醇的快速挥发, 孔隙分布均匀且相互连通. 随烧结温度升高, 气孔率、开气孔率和比表面积分别由77.8%、76.0%和10.39m²/g下降到67.6%、65.5%和4.26m²/g, 而抗压强度则由3.29MPa显著提高到32.36MPa, 材料孔径大小受烧结温度影响较小, 孔径尺寸呈单峰分布, 且几乎所有的气孔都为开口气孔, 透气度与孔径尺寸具有一致的变化关系. 莫来石多孔陶瓷在高气孔率条件下仍然保持高强度的主要原因是材料中均匀的孔隙结构、孔径尺寸小且相对集中、以及因烧结颈的形成在空间上所表现出的一种颗粒搭接骨架结构.     

低介电常数多孔氮化硅陶瓷的制备

采用凝胶注模成型工艺,以SiO2含量大于等于95%的空芯玻璃微珠作造孔剂,通过控制造孔剂的加入量和调节造孔剂的孔径成功制备出低介电常数、高强度的多孔Si3N4陶瓷。结果表明,随着造孔剂含量的增加,试样气孔率增大,弯曲强度降低,ε和tanδ都相应降低,ε最低为1.77;在造孔剂加入量为10%时,随着造孔剂的孔径尺寸变大,试样的孔径变大,弯曲强度降低,试样的ε和tanδ也相应降低。当造孔剂含量为10%、孔径尺寸为80μm时制备的多孔氮化硅陶瓷ε为2.13,弯曲强度达到38MPa,适合作为宽频带天线罩的夹层材料。     

玻璃粉基空心微珠多孔材料的吸声性能研究

采用低成本的通过废玻璃制备的空心微珠坯体为原料,经过低温烧结制备一种超轻高强多孔材料,研究了烧结温度、保温时间对样品孔结构和吸声性能的影响。结果表明,随着烧结温度的升高,样品的平均孔径尺寸逐渐增大,保温时间越长,样品的开孔气孔率越大;开孔气孔率越大,样品吸声性能越好;样品平均孔径尺寸的变化显著影响在中高频段的吸声性能,平均孔径尺寸为2.51mm的样品,对于频率为1 000Hz的声波,吸声系数可达0.84。空心微珠多孔材料的平均吸声系数随着流阻的增大先增大后减小,当流阻值达到4.805×105 Pa·s/m3时,样品吸声性能最佳。     

融盐自发浸渗用微米级多孔陶瓷预制体的烧制

探索以SiO2为骨料,选择合适的助剂、烧成制度、成型压力和颗粒粒度,烧制成三维连通网格状多孔陶瓷预制体的工艺制度,用于自发浸渗熔融无机盐相变材料以制备无机盐/陶瓷基复合相变储能材料.讨论了制备工艺与预制体的显气孔率、孔结构以及显微组成之间的关系,烧制出的石英质多孔陶瓷具有40%～45%的显气孔率和5～40μm的孔径大小,完全符合自发熔融浸渗工艺的要求.     

用于过滤膜的梯度孔径Ni-Cr-Fe多孔材料的制备及性能

本工作采用元素粉末反应合成法,利用固相偏扩散的原理进行固相烧结制备Ni-Cr-Fe多孔材料支撑体,再利用人工刷涂的方法将同配比且较细的Ni、Cr、Fe元素粉末悬浮浆料刷涂于多孔支撑体表面,经过真空烧结,制备得到梯度孔径Ni-Cr-Fe多孔材料。通过XRD、SEM、能谱等测试手段表征烧结后的梯度孔径Ni-Cr-Fe多孔材料的物相及孔结构性能。结果表明,同质的梯度孔径Ni-Cr-Fe多孔材料膜层完整,结合强度较好,以冶金桥接的方式结合。随着膜层厚度的增加,透气度将减小,当过渡层的厚度为80μm,表面膜层厚度为30μm时,最大孔径为6μm,透气度为936 m~3·m~(-2)·h~(-1)·kPa~(-1),透气度下降22. 64%。在膜层等厚且过滤精度达到要求时,二阶梯度孔径Ni-Cr-Fe多孔材料透气度的下降率比一阶梯度孔径NiCr-Fe多孔材料透气度的下降率小。过渡膜层起到了非常关键的作用,实现了在较高过滤精度的基础上具有较大的过滤通量。     

酚醛树脂聚合相分离热解制备介孔碳

采用酚醛树脂聚合相分离热解制备多孔碳, 用压汞仪和场发射扫描电镜对多孔碳性能进行表征, 同时研究了固化催化剂含量对多孔碳性能的影响. 实验结果表明, 制备得到的多孔碳的孔呈交联互通状且孔径分布较窄, 大部分孔分布在20～50nm之间. 多孔碳的平均孔径约40nm. 高固化催化剂含量使多孔碳具有更薄的孔壁及更高的显气孔率. 当固化催化剂含量为15%时, 多孔碳的显气孔率为54.3%. 胶凝速度以及体积收缩是改变多孔碳性能的两个因素.     

复杂结构的压电陶瓷成型工艺研究

快速成型和凝胶注模的有机结合是制备复杂结构陶瓷体的有效方法,该工艺的关键是制备高固相、低黏度的注模浆料.采用快速成型和凝胶注模制备复杂结构的PMN-PZT压电陶瓷,重点讨论了分散剂、浆料pH值和球磨时间对注模浆料黏度的影响,并对该工艺和传统模压成型工艺制备的样品进行了形貌分析和电学性能测定.结果表明:当分散剂用量在0.9%~1.1%,pH值为10.5~11.5,球磨时间为8 h时,可以制备出固相含量为55%,黏度小于1 Pa.s的压电陶瓷浆料.使用该浆料制备的复杂结构压电陶瓷体与模压成型工艺相比,显微结构均匀致密、晶粒大小与晶界分布均匀,气孔率更小,电学性能更均匀.     

凝胶浇注结合固相烧结制备具有多级孔结构的碳化硅陶瓷

以Isobam作为胶凝剂, 聚甲基丙烯酸甲酯(PMMA)作为泡沫稳定剂和造孔剂, 结合固相烧结制备出具有多级孔结构的碳化硅陶瓷, 并研究了PMMA添加量、球磨机转速以及烧结温度对多孔陶瓷结构及性能的影响。结果表明: 当球磨机转速为220 r/min、烧结温度为2100℃时, 随着PMMA添加量由5wt%增加到20wt%, 发泡过程受到抑制, 但是泡沫的稳定性增强, 所得多孔陶瓷的气孔率在51.5%~72.8%之间, 压缩强度介于7.9~48.2 MPa之间; 当PMMA加入量为20wt%时, 随着球磨机转速由220 r/min增大到280 r/min, 加剧了浆料的发泡过程, 2100℃烧结所得多孔陶瓷的气孔率逐步增大, 气孔孔径变大; 当球磨机转速为220 r/min, PMMA加入量为20wt%时, 随着烧结温度的升高, 气孔率逐渐降低, 力学性能有所提高。     

发泡法制备多孔镁合金的研究

本文采用熔体发泡法制备以MgCO_3为发泡剂的AZ91D多孔镁合金。研究了不同的发泡温度对试样的显微组织、孔隙率、真密度及硬度的影响。结果表明:随着发泡温度的提高,β相的网状结构开始破碎,孔隙率呈现出增大趋势,但平均孔径逐渐减小;在不同的发泡温度下,AZ91D多孔镁合金的孔隙率大致保持在37%~50%之间,真密度变化范围为0.9~1.9 g/cm~3之间,发泡温度为720℃时,所得到的多孔试样的孔分布比较均匀,且孔隙率最大;随着发泡温度的增加,合金试样的硬度值减小,但下降幅度较小。     

Effects of surfactants on the microstructure of porous ceramic scaffolds fabricated by foaming for bone tissue engineering

A porous scaffold comprising a β-tricalcium phosphate matrix and bioactive glass powders was fabricated by foaming method and the effects of surfactants as foaming agent on microstructure of scaffolds were investigated. Foaming capacity and foam stability of different surfactants in water firstly were carried out to evaluate their foam properties. The porous structure and pore size distribution of the scaffolds were systematically characterized by scanning electron microscopy (SEM) and an optical microscopy connected to an image analyzer. The results showed that the foam stability of surfactant has more remarkable influence on their microstructure such as pore shape, size and interconnectivity than the foaming ability of one. Porous scaffolds fabricated using nonionic surfactant Tween 80 with large foam stability exhibited higher open and total porosities, and fully interconnected porous structure with a pore size of 750-850 μm.     

碳酸钙对磷渣-煤矸石烧结多孔微晶玻璃结构和性能的影响

多孔微晶玻璃具有导热系数低、力学性能好、抗腐蚀性强等优点,是一种隔热、吸声的轻质功能材料。为拓展多孔微晶玻璃的制备原料范围,同时大宗量、高附加值利用工业废渣-磷渣和煤矸石。本文以磷渣和煤矸石为原料,采用烧结法制备多孔微晶玻璃。利用X射线衍射、扫描电子显微镜及阿基米德法,对制备的试样进行表征,研究发泡剂碳酸钙掺量对体系析晶、发泡和宏观性能的影响。研究表明,碳酸钙掺量不影响体系析晶相的种类,但体系析晶度随碳酸钙掺量增加先增大后减小;碳酸钙掺量为2%~6%(质量分数)时,增大掺量,利于发泡。体系中气孔孔径增大且趋于均匀,试样孔隙率增大,体积密度降低。但随着掺量进一步增大,体系发泡效果降低。当碳酸钙掺量为4%~8%(质量分数)时,可获得体积密度为0.86~0.92 g/cm³,孔隙率为60.7%~70.3%,抗压强度为7.89~15.11 MPa,性能较优的硅灰石多孔微晶玻璃。本研究以工业废渣为原料,降低了多孔微晶玻璃的制备成本,同时为工业废渣利用提供一种途径借鉴,具有深远的资源和环保意义。     

多孔青铜过滤片的制备工艺及结构特性探究

开发一种工艺简单、重复性好、孔形孔径易控制、制取成本低的铜基多孔材料制备工艺是当前的研究热点之一.本文以青铜粉为原料,K_2CO_3为造孔剂,采用烧结溶解法制备多孔青铜过滤片,研究了造孔剂、烧结温度对样品孔隙率的影响,分析了烧结温度、压制压力对样品最大孔径和透气系数的影响,以及孔隙率与抗压强度的关系.研究结果表明:当造孔剂体积分数为20%~40%时,所制备样品的孔隙率为22.8%~44.4%,开孔孔隙率为18.5%~37.2%;随着烧结温度的升高,样品孔隙率和透气系数下降;随着压制压力增加,最大孔径和透气系数均减小;随着样品孔隙率增大,抗压强度减小.当选择造孔剂体积分数30%、压制压力150 MPa、烧结温度800℃的工艺参数下,制备出孔隙率32.2%、最大孔径4.6μm、透气系数9.27 m~3/(h·k Pa·m~2)、压缩强度27.9 MPa的多孔青铜过滤片.     

Pore structure of porous ceramics synthesized from water-based slurry by freeze-dry process

A unique porous ceramic with complex pore structure was synthesized by the freeze-dry process. A water-based ceramic slurry was frozen while controlling the growth direction of ice, and sublimation of the ice were generated by drying it at a reduced pressure. By sintering this green body, a porous ceramic with complex pore structure was obtained, where macroscopically aligned open pores exceeding 10 m in size contained minute pores of about 0.1 m in their internal walls. Wide control of the porosity was possible by changing the concentration of the starting slurry. The pore size distribution as well as the microstructure were substantially affected by the freezing and sintering temperatures. Optimization of the synthesis conditions was investigated in order to obtain the desired pore structure.     

莰烯基冷冻浇注成型法制备定向通孔氧化铝陶瓷

由莰烯、氧化铝、Texaphor 963组成的陶瓷料浆,在温度梯度的诱导下,用冷冻浇注成型法制备了氧化铝陶瓷坯体,经干燥、烧结后,制备出了高孔隙率、高强度的定向通孔氧化铝陶瓷.通过扫描电镜观察其孔结构,并对其孔隙率、抗压强度和收缩率进行分析测试.结果表明:料浆的固体含量和烧结温度显著影响试样的气孔率、抗压强度和收缩率;...     

Thermo-mechanical stability of porous alumina: effect of sintering parameters

Recently, we proposed a two-step heating schedule involving pulse electric current sintering (PECS), a kind of pressure assisted vacuum sintering, and subsequent post-heat treatment in air to fabricate porous alumina support, using commercially available alumina and carbon powders [J. Mater. Res. 18 (2003) 751]. During pressure assisted vacuum sintering, Al₂O₃–C system of low porosity was obtained and in second stage, i.e. during post-heat treatment in air, carbon particles present in the Al₂O₃–C system burnt out to form highly porous Al₂O₃ support. Following our previous brief study, the effects of sintering parameters such as temperature, pressure, and heating rate on the properties of the porous alumina were investigated. The porosity varied between 28 and 38% depending on the sintering parameters. As desired, the pore size distribution did not change with post-heat treatment temperature and hence the mechanical properties as well. It was concurred from this present study that the sintering parameters of PECS greatly influenced pore characteristics and other properties of porous compacts. We admit that the initial composition ratio of powder mixture (Al₂O₃:C) also plays important role on properties such as porosity, pore size, etc. which is beyond the scope of this present study.     

Control of morphological properties of porous biodegradable scaffolds processed by supercritical CO2 foaming

A low cost supercritical CO₂ foaming rig with a novel design has been used to prepare fully interconnected and highly porous biodegradable scaffolds with controllable pore size and structure that can promote cancellous bone regeneration. Porous polymer scaffolds have been produced by plasticising the polymer with high pressure CO₂ and by the formation of a porous structure following the escape of CO₂ from the polymer. Although, control over pore size and structure has been previously reported as difficult with this process, the current study shows that control is possible. The effects of processing parameters such as CO₂ saturation pressure, time and temperature and depressurisation rate on the morphological properties, namely porosity, pore interconnectivity, pore size and wall thickness- of the scaffolds have been investigated. Poly(d,l)lactic acid was used as the biodegradable polymer. The surfaces and internal morphologies of the poly(d,l)lactic acid scaffolds were examined using optical microscope and micro computed tomography. Preosteoblast human bone cells were seeded on the porous scaffolds in vitro to assess cell attachment and viability. The scaffolds showed a good support for cell attachment, and maintained cell viability throughout 7 days in culture. This study demonstrated that the morphology of the porous structure can be controlled by varying the foaming conditions, allowing the porous scaffolds to be used in various tissue engineering applications.     

粉末冶金法制备多孔金属钛免疫隔离材料

采用粉末冶金工艺制备出微米孔径且孔隙率较高的多孔钛免疫隔离材料，分析了压制压力、烧结温度等因素对多孔金属钛孔径及孔隙率的影响。试验结果表明，随着压制压力的提高，钛粉末烧结后平均孔径尺寸和孔隙率逐渐减小，孔隙分布和孔径尺寸较均一。烧结温度对多孔金属钛影响显著，随烧结温度的升高，平均孔径尺寸逐渐增大，孔隙率先略有上升后逐渐降低。