多孔陶瓷制备技术的进展

多孔陶瓷是一种含有较多孔隙的无机功能材料,在化工、冶金、运输等领域有着广泛的应用前景.对多孔陶瓷的制备技术及最新研究进展进行了详细的综述,报道了一种在自蔓延高温合成法和发泡法基础上创新的制备方法--自蔓延高温合成喷射法,并对未来研究方向进行了展望,认为今后对多孔陶瓷制备技术的研究将沿着对现有技术进行改进及结合其他种类材料的制备技术进行创新等两个方向开展.     

泡沫注凝法制备刚玉-莫来石多孔陶瓷

以T60板状刚玉粉(d50=10.74μm)、ZTP-200氧化铝微粉(d50=4.96μm)、RG4000煅烧氧化铝微粉(d50=1.46μm)和NS-30型硅溶胶为原料,采用泡沫注凝法制备了刚玉-莫来石多孔陶瓷,主要研究了粉料粒度级配(d50分别为1.46、4.96、10.74μm的三种氧化铝粉料的质量分数分别为44%、26%、30%,36%、28%、36%,30%、29%、41%,21%、29%、50%)和浆料中硅溶胶加入量(质量分数分别为0、2%、4%)对坯体的烧后收缩及烧后试样的致密度、常温耐压强度、热导率、相组成和显微结构的影响。结果表明:1)d50=10.74μm的粗颗粒加入量增加,试样的烧后线收缩率、致密度和常温耐压强度减小;2)硅溶胶加入量增加,试样的烧后线收缩率和体积密度减小,但由于SiO2与Al2O3反应生成莫来石,试样的常温耐压强度变化较复杂;3)泡沫注凝法制备的刚玉-莫来石复相多孔陶瓷具有球形孔结构,平均孔径约为140μm,其性能如下:烧后线收缩率9.29%,体积密度0.78 g·cm-3,显气孔率79.8%,常温耐压强度25.3 MPa,1 000℃(热面温度)下的热导率为0.481W·m-1·K-1。     

多孔陶瓷材料的制备研究进展

介绍了多孔陶瓷材料的分类、性能和应用,综述了多孔陶瓷的制备方法,并分析了不同制备方法的特点。     

The preparation and characterization of porous alumina ceramics using an eco-friendly pore-forming agent

This work presents the preparation of porous alumina ceramics through the sacrificial phase method, using an eco-friendly material, namely waste coffee grounds, as a pore-forming agent. The effects of coffee grounds content in the green ceramic bodies on the linear and volumetric shrinkage, as well as the total and open porosity of the sintered product, were evaluated. The influence of the resulting porosity on mechanical properties of the prepared porous alumina was determined using Brazilian disk compression test for the determination of the indirect tensile strength of the prepared samples. Microstructure and pores morphology were characterized by scanning electron microscopy. Porosities in the range 35-54 vol% were achieved, by varying the coffee grounds content from 0 to 50 wt% in the green bodies. The indirect tensile strength of the final obtained porous alumina ceramic decreased accordingly from 57.4 MPa to 17.7 MPa.     

叔丁醇基凝胶注模成型制备氧化铝多孔陶瓷

以微米级Al2O3粉料为原料,叔丁醇为溶剂,采用凝胶注模成型工艺制备了氧化铝多孔陶瓷,并研究了Al2O3浆料的固相体积分数(分别为8%、10%、13%和15%)对1 500℃保温2 h烧后氧化铝多孔陶瓷的气孔率、气孔孔径分布、耐压强度、热导率和显微结构的影响.结果表明:当Al2O3浆料的固相体积分数从8%增加到15%时,氧化铝多孔陶瓷烧结体的总气孔率从71.2%逐渐降低至61.2%,气孔平均孔径从1.0 μm逐渐减小至0.78 μm,耐压强度从16.0 MPa逐渐增大至45.6 MPa,而热导率从1.03 W·(m·K)-1逐渐增大至1.83W·(m·K)-1.     

Preparation and properties of magnesia porous ceramics by particle-stabilized foam casting

In this paper, magnesia porous ceramics were prepared by particle-stabilized foams assisted foam-gel casting. Secondly, the performance of magnesia slurry and magnesia porous ceramics was investigated. The obtained magnesia powder manifested high adsorption amount and excellent hydrophobicity, due to the strong adsorption ability of sodium dodecyl benzene sulfonate (SDBS) on magnesia particles. When the SDBS concentration is .3 wt%, the surface tension and expansion ratio of the slurry were 45 mN·m⁻¹ and 1.68, respectively. The shape of the pore was sphere cell structure, with uniform distribution of pores in the sample, the average pore size was in the range of 58.7–73.9 μm, and the compressive strength was in the range of 25.3 MPa to 15.5 MPa when porosity varied from 56.7% to 70.2%.     

生物SiC多孔陶瓷的研究进展

介绍了生物SiC多孔陶瓷的研究现状,并对生物碳模板的分类、制备方法进行了详尽的叙述,同时对生物SiC多孔陶瓷的各项性能进行了综述,最后对生物SiC多孔陶瓷的发展趋势作了总结。     

Preparation of elongated mullite self-reinforced porous ceramics

Elongated mullite was synthesized using mullite powder as a raw material and AlF₃·3H₂O as an additive, and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The effects of AlF₃·3H₂O content and reaction temperature on the formation of elongated mullite were investigated, and the relevant growth mechanism was discussed based on the experimental results and density functional theory (DFT) calculations. When the optimal amount of AlF₃·3H₂O (4?wt% in the present work) was used, the length and diameter of elongated mullite increased with increasing the reaction temperature, and elongated mullite of 22.3?µm in average length and 4.6?µm in average diameter was formed after 5?h at 1873?K. Based on the results, elongated mullite self-reinforced porous ceramics were prepared by a combined foam-gelcasting and solid-reaction method, and their mechanical properties were examined. Elongated mullite in-situ formed in the porous samples evidently enhanced their mechanical strength. The flexural strength of the elongated mullite self-reinforced porous sample with 67.0% porosity (prepared using 6?wt% AlF₃·3H₂O) was as high as 13.9?MPa, which was about 26.4% higher than that of a porous sample (11.0?MPa) prepared without AlF₃·3H₂O.     

Near net shape fabrication of porous cordierite by combination of foam gel-casting and freeze-drying

Near net shape fabrication of porous cordierite was successfully achieved through a combination of foam gel-casting, freeze-drying, and in situ synthesis. Environment friendly gelation was used as gel system, and the gelatin concentration influenced the drying shrinkage vastly. Combined with the volume expansion coming from phase transition and solid reaction during in situ synthesis of cordierite, the total linear shrinkage could be controlled around zero (−1.87% to 0.45%) by adjusting the gelation concentration and solid content in the slurry, meanwhile the prepared porous cordierite ceramics showed both high porosity (85.9%–91.1%) and high compressive strength (0.58–3.37 MPa). The sample with 0.05 g/ml gelatin concentration and 20 vol% solid content possessed excellent performance: total porosity of 89.1%, compressive strength of 1.36 MPa, and specific strength of 4.9 MPa/(g/cm³), showing the potential usage of filter carrier.     

Tailored pore structures and mechanical properties of porous alumina ceramics prepared with corn cob pore-forming agent

In this work, the effects of porosity and different particle sizes of pore-forming agent on the mechanical properties of porous alumina ceramics have been reported. Different grades of porous alumina ceramics were developed using corn cob (CC) of different weight contents (5, 10, 15, and 20 wt%) and particle sizes (<63 µm, 63-125 µm and 125-250 µm) as the pore-forming agent. Experimental results showed that total porosity and pore cavity size of the porous alumina ceramics increased with rising addition of CC pore former. Total porosity increased with increasing particle size of CC with the Al₂O₃-^<63CC₅ sample exhibiting the lowest total porosity of 41.3 vol% while the highest total porosity of 68.1 vol% was exhibited by the Al₂O₃-^125-250CC₂₀. The particle size effect of CC on the mechanical properties revealed that diametral tensile strength and hardness of the porous alumina ceramics deteriorated with increasing particle size of CC pore former. The Al₂O₃-^<63CC₅ sample exhibited the highest diametral tensile strength and hardness of 25.1 MPa and 768.2 HV, respectively, while Al₂O₃-^125-250CC₂₀ exhibited the lowest values of 1.1 MPa and 35.9 HV. Overall, porous alumina ceramics with the smallest pore sizes under each particle size category exhibited superior mechanical properties in their respective categories.     

Low sintering shrinkage porous mullite ceramics with high strength and low thermal conductivity via foam-gelcasting

Excessive sintering shrinkage leads to severe deformation and cracking, affecting the microstructure and properties of porous ceramics. Therefore, reducing sintering shrinkage and achieving near-net-size forming is one of the effective ways to prepare high-performance porous ceramics. Herein, low-shrinkage porous mullite ceramics were prepared by foam-gelcasting using kyanite as raw material and aluminum fluoride (AlF₃) as additive, through volume expansion from phase transition and gas generated from the reaction. The effects of AlF₃ content on the shrinkage, porosity, compressive strength, and thermal conductivity of mullite-based porous ceramics were investigated. The results showed that with the increase of content, the sintering shrinkage decreased, the porosity increased, and mullite whiskers were produced. Porous mullite ceramics with 30 wt% AlF₃ content exhibited a whisker structure with the lowest shrinkage of 3.5%, porosity of 85.2%, compressive strength of 3.06 ± 0.51 MPa, and thermal conductivity of 0.23 W/(m·K) at room temperature. The temperature difference between the front and back sides of the sample reached 710°C under high temperature fire resistance test. The low sintering shrinkage preparation process effectively reduces the subsequent processing cost, which is significant for the preparation of high-performance porous ceramics.     

Effect of alumina fiber content on pore structure and properties of porous ceramics

Porous Al₂O₃ ceramics with different contents of alumina fibers were prepared by gel-casting process. The effects of Al₂O₃ fiber content on pore size distribution, porosity, compressive strength, and load-displacement behavior of the ceramic materials were investigated. Initial results showed that with the increase of Al₂O₃ fiber content, the pore size and porosity of the material is increased, and the compressive strength is decreased. However, upon increasing the fiber content from 50 wt% to 67 wt%, the performance of the samples changed greatly. The compressive strength of the material increased, while the porosity remained unchanged, the pore size increased greatly, and the shape of the load displacement curve changed. It showed that when the fiber content increased from 50 wt% to 67 wt%, the loading body in the fiber-reinforced porous ceramics changed from particles to fibers.     

含镁铝尖晶石的铝酸盐水泥的制备与应用

按天然白云石(≤0.1mm)与工业氧化铝粉(≤0.088mm)的质量比为45∶55配料,经混合、成型和烘干后,于1600℃3h煅烧,细磨烧结体得到含镁铝尖晶石的新型铝酸盐水泥。测量了新型铝酸盐水泥的凝结时间、耐火度以及用其所结合高铝矾土制成的耐火浇注料的早期强度;利用XRD、SEM和EDS分析了新型铝酸盐水泥的物相组成及其形貌和分布,同时采用静态坩埚法对比了新型铝酸盐水泥和纯铝酸钙水泥结合刚玉浇注料的抗渣性差异。结果表明:新型水泥的物相组成为镁铝尖晶石(MA)、一铝酸钙(CA)和二铝酸钙(CA2),且这3个物相的分布较为均匀;新型水泥的凝结时间正常,耐火度高于纯铝酸钙水泥;用新型水泥制得的刚玉浇注料抗渣性好;其原因是新型水泥组成中引入了镁铝尖晶石相,而镁铝尖晶石具有较高的熔点和抗熔渣侵蚀能力。     

Near-net-size preparation of porous mullite matrix ceramics with in situ formed 3D mullite whisker network

Porous mullite matrix ceramics have excellent thermal and mechanical properties suitable for applications such as in thermal insulation. However, their applications are limited by processing defects from nonuniform sintering shrinkage and the trade-off between high porosity (preferred for low thermal conductivity) and high mechanical strength. Herein, we seek to minimize the sintering shrinkage by near-net-size preparation and improve the strength by in situ formed whisker network structure. Gelcasting forming technology and pressureless sintering were used to prepare porous mullite matrix ceramics using kyanite and α-Al₂O₃ powders as the starting materials and using MoO₃ to promote the growth of mullite whiskers. The results showed that the sintering shrinkage could be compensated by the volume expansion from solid-state reaction during reaction sintering. The in situ formed three-dimensional (3D) whisker network further reduced sintering shrinkage and effectively improved the strength of the ceramics. An ultralow sintering shrinkage of .78% was achieved. The near-net-shape porous mullite matrix ceramics strengthened by 3D whisker network had a high porosity of 63.9%, a high compressive strength of 83.8 MPa and a high flexural strength of 53.5 MPa.     

Preparation and properties of porous Al2O3-based ceramics by gel casting using MgO as a gelling and consolidating agent

Low-cost and environment-friendly MgO was used as a new gelling and consolidating agent to fabricate porous Al₂O₃-based ceramics via a gel casting routine. Effects of 800°C calcined additions of MgO (.5, 1.0, 1.5, and 2.0 wt%, respectively) on open porosity (OP), pore size distribution, gas flux, and microstructure of the porous ceramics were investigated deliberately. The experimental results showed that 800°C calcined MgO exhibits excellent gelling and consolidating performance at 80°C, mainly owing to the hydration reaction between MgO and H₂O and thus results in high-quality porous Al₂O₃-based ceramics without deformation and cracking. The Al₂O₃–water suspensions with different MgO additions have good flowability at room temperature. Moreover, water absorption, open porosity, and gas flux of the as-prepared porous ceramics increase remarkably with rising of MgO addition. Furthermore, MgO addition significantly suppresses the abnormal growth of Al₂O₃ grains, and thus the microstructure of the porous Al₂O₃-based ceramics becomes more uniform. This technique of gel casting using MgO as a new gelling and consolidating agent offers an alternative routine for a large-scale production of porous ceramics.     

颗粒级配对发泡法-凝胶注模制备Al_2O_3多孔陶瓷性能的影响

为了降低Al2O3多孔陶瓷制备过程中的干燥后收缩和烧后收缩,提高成品率,将d50分别为25.1、9.4和1.1μm的粗、中、细Al2O3粉体按粗粉中粉细粉质量比分别为50 40 10、10 40 50和100%全细粉的级配方式制备Al2O3泡沫浆料,研究颗粒级配对浆料黏度、干燥生坯的线收缩、烧后试样的线收缩、烧后试样的热导率等性能的影响。结果表明:颗粒级配可以有效提高固含量,且颗粒级配后的发泡浆料在静置30 min后仍能保持稳定,颗粒级配可以明显降低生坯的干燥线收缩以及烧后线收缩,并能降低热导率,提高了发泡法-凝胶注模工艺制备氧化铝多孔陶瓷的成品率。     

Preparation of calcium hexaluminate porous ceramics by gel-casting method with polymethyl methacrylate as pore-forming agent

Calcium hexaluminate (CA₆) porous ceramics were prepared by gel-casting method, with α-Al₂O₃ and CaCO₃ as raw materials and polymethyl methacrylate (PMMA) microspheres as pore-forming agent. The effects of the amount of pore-forming agent PMMA microspheres on the phase composition, bulk density, apparent porosity, flexural strength, microstructure, thermal shock stability and thermal conductivity of CA₆ porous ceramics were systematically studied. The pores of CA₆ porous ceramics are mainly formed by the burning loss of PMMA microspheres and the decomposition of organic matter. Adding an appropriate amount of PMMA microspheres as pore-forming agent has a positive effect on the thermal shock stability of CA₆ porous ceramics. When the amount of pore-forming agent is 15 wt%, the volume density of CA₆ porous ceramics is 1.33 g/cm³, the porosity is 63%, the flexural strength is 13.9 MPa, the thermal shock times can reach 9 times, and the thermal conductivity is 0.293 W/(m·K), which can meet the application in refractory, ceramics or high temperature cement industries.     

多孔陶瓷为载体的C3馏分选择加氢催化剂的研究

采用氧化铝涂层改性后的多孔陶瓷为载体，制备以钯为活性组分的C₃馏分选择性加氢催化剂。该载体可提供较大的比表面积，催化剂活性组分负载均匀。微反实验结果表明，制备的催化剂具有较高的C₃馏分选择加氢活性和选择性。     

淀粉燃料对多孔Al_2O_3-ZrO_2(Y_2O_3)陶瓷性能的影响

为了提高多孔Al2O3-ZrO2(Y2O3)陶瓷的强度,以尿素和淀粉为燃料,用低温燃烧法合成活性较高的Al2O3-ZrO2(Y2O3)复合粉体,并用此粉体制备了多孔Al2O3-Zr O2(Y2O3)陶瓷,研究燃烧前驱体中淀粉的外加量(质量分数分别为0、15%、25%、35%、45%、55%)对多孔陶瓷显气孔率、抗折强度和显微结构的影响。结果表明:与尿素为燃料相比,以尿素和淀粉为燃料能提高复合粉体的烧结活性,有效改善多孔陶瓷的显微结构,提高多孔陶瓷的抗折强度。     

Direct foaming of Al2O3-based macroporous ceramics containing pre-foamed colloidal alumina,calcite and CAC suspension

Adding pre-foamed colloidal alumina to ultrastable Al₂O₃-stabilised foams can be a path towards partially counteracting the firing shrinkage of these materials and producing macroporous ceramics with smaller pores. Nevertheless, this system still presents a long setting time and high sintering-induced shrinkage, which hinders the production of larger samples and reduces its porosity. In the present work, it was observed that adding calcium aluminate cement suspension (CAC_S) and CaCO₃ (calcite) to the aforementioned system can speed up its solidification kinetics, improve its mechanical strength and reduce its shrinkage after firing, maintaining high porosity and smaller pore sizes. By using these raw materials, samples with an average pore size below 60 μm, total porosity above 70%, and a narrower pore size distribution were attained after thermal treatment at 1600 °C for 5h. Moreover, due to the in situ formation of calcium hexaluminate, their shrinkage after sintering was almost halved (from ~20% to 11%).