氧化铝/莫来石复合泡沫陶瓷的制备研究
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摘要
泡沫陶瓷是一种特殊工艺制作的开孔率高达70%～90%并具有三维立体网络骨架结构和贯通气孔的新型多孔陶瓷材料,具有化学性能稳定、强度高、耐高温、抗热震性好、比表面积大等诸多优点。其中的氧化铝/莫来石复合泡沫陶瓷材料以制备成本低、使用功效高而受到业内广泛关注。
针对普通粘土质泡沫陶瓷强度较低、抗热震性能差、适用范围小等缺点;单组分SiC、AlN、ZrO_2等泡沫陶瓷烧结温度高、成本高昂等现状,作者以氧化铝/莫来石复合泡沫陶瓷的制备为研究对象,采用有机泡沫浸渍法制备了氧化铝/莫来石复合泡沫陶瓷,系统研究了各种因素对该材料性能的影响,获得了如下研究成果。
(1)有机泡沫前驱体预处理能显著提高浸浆量。实验选用聚氨酯海绵为有机前驱体,聚氨酯海绵经碱处理后破坏了聚氨酯海绵的网络间膜,同时也增加了茎的粗糙度,一定程度上改善了浸浆性能;而经过碱处理再经CMC改性的海绵与浆料润湿性得到了改善,聚氨酯海绵的浸浆量增加。
(2)研究发现,在浆料中加入适当的分散剂可获得高固相含量、均匀稳定、流变性良好、适于浸渍的浆料。实验结果表明,浆料中加入质量分数为0.4%的分散剂聚丙烯酸胺获得的浆料性能最优;固含量为68.4%～69.4%时最适合浸渍;对辊间距与前驱体浸浆量的关系紧密,较佳的d/h(其中d为对辊间距,h为海绵高度)控制范围为9.45%～10.35%。
(3)微波干燥提高了复合泡沫陶瓷的抗压强度和成品率。实验采用微波干燥方式有效地减少了椭圆变形,增加了浸浆量的限制范围,因此,泡沫陶瓷制品的抗压强度和成品率得到提高,同时提高了干燥效率,节约了能源。
(4)通过对不同配方陶瓷烧结温度的研究,分析得到烧结过程中陶瓷物相的演变,同时考察了烧结温度对陶瓷性能的影响,得出配方B为最佳配方;通过对配方B陶瓷不同烧结保温时间的研究,得到了保温时间对复合泡沫陶瓷性能的影响,实验确定复合陶瓷较佳的烧结温度为1500℃,保温时间为90min,该工艺条件制备的复合泡沫陶瓷开孔率达到81.2%,抗压强度达到1.21MPa,抗热震性能(D_(st))为0.52。
(5)研究发现,添加Y_2O_3、CaO不仅能有效促进氧化铝/莫来石复合泡沫陶瓷材料的烧结,提高陶瓷致密度,而且还能够显著提高复合泡沫陶瓷的抗压强度和抗热震性能。
采用上述方法所制备的复合泡沫陶瓷材料不仅能较好地解决普通泡沫陶瓷强度低,抗热震性能差的问题,而且制备成本低,绿色环保,具有较好的工业应用前景。
Ceramic foam with high porosity (70%-90%)and a structure of open cells in a three-dimensional network is a new type porous ceramics material made by special technique. It has many good performances such as good chemical stability, high intensity, high temperature resistance, good thermal shock resistance, large specific surface area, and so on. Because of the low cost and high efficacy, alumina-mullite ceramic foams has been widely concerned in the industry.
According to those disadvantages of ordinary clayey foam ceramics, such as low strength, low thermal shock resistance, and narrow scope of application, and the high production temperature and high cost of ceramic foams which have single component such as SiC, AlN and ZrO_2, We carried on the study on the preparation of alumina-mullite ceramic foams with polymer-sponge method, gave a systematic research on the effect of different factors on the performance of material. The research results are as follow:
(1) Pre-treatment of polymer foam increased the grouting-absorption capacity of polymeric sponge. Choose the polymeric sponge as the precursor of ceramic foams. Through alkali treatment, the film of polymeric sponge between stalks was destroyed, and the roughness of the polymeric sponge surface roughness can be increased. And then with CMC modification added, the wetting ability and grouting-absorption capacity of polymeric sponge were increased.
(2) Through adding appropriate dispersant, we can obtain the slurry with high solid content, good equality and stabilization, and excellent rheology. It was found that the best aqueous slurry can be obtained by adding 0.4% quality content PMAA-NH_4. And the slurry was most suitable for the impregnation when solid content was between 68.4%-69.4%. The gap of two-parallel rolls has a closed relationship with the grouting-absorption capacity of precursor. The best d/h(d- the distance of the gap of two-parallel rolls, h-height of polymeric sponge) was 9.45%-10.35%.
(3) The compressive strength and yield of complex ceramic foams was increased by microwave drying method. By microwave drying method, elliptical deformation was reduced effectively and the limit of grouting-absorption capacity was enlarged. So the compressive strength and yield of ceramic foams was increased. Moreover it increased the drying efficiency, and saved the energy.
(4) According to the research on the sintering temperature of ceramic with different recipe, the evolution of ceramic phase was studied. Through observing the effect of sintering temperature on ceramic performance, the best recipe B was finally confirmed. By studying on different sinter-holding time with recipe B, the influence of holding time on ceramic foam performance was obtained. The optimum sintering temperature of alumina-mullite ceramic foam was determined as 1500℃, and the optimum holding time was 90min. Under this condition, the porosity of alumina-mullite ceramic foam product was increase to 81.2%, the compressive strength was 1.21Mpa, and the thermal shock resistance (D_(st)) was 0.52.
(5) It was found that additives Y_2O_3 and CaO had a promoting effect on the sintering and density improving of alumina-mullite ceramic foams. Moreover, they could improve the compressive strength and thermal shock resistance greatly.
Prepare composite ceramic foam with above method can not only solve the problem of low strength and thermal shock resistance, but also reduce the cost and be environmental. It has good prospect for industrial application.
针对普通粘土质泡沫陶瓷强度较低、抗热震性能差、适用范围小等缺点;单组分SiC、AlN、ZrO_2等泡沫陶瓷烧结温度高、成本高昂等现状,作者以氧化铝/莫来石复合泡沫陶瓷的制备为研究对象,采用有机泡沫浸渍法制备了氧化铝/莫来石复合泡沫陶瓷,系统研究了各种因素对该材料性能的影响,获得了如下研究成果。
(1)有机泡沫前驱体预处理能显著提高浸浆量。实验选用聚氨酯海绵为有机前驱体,聚氨酯海绵经碱处理后破坏了聚氨酯海绵的网络间膜,同时也增加了茎的粗糙度,一定程度上改善了浸浆性能;而经过碱处理再经CMC改性的海绵与浆料润湿性得到了改善,聚氨酯海绵的浸浆量增加。
(2)研究发现,在浆料中加入适当的分散剂可获得高固相含量、均匀稳定、流变性良好、适于浸渍的浆料。实验结果表明,浆料中加入质量分数为0.4%的分散剂聚丙烯酸胺获得的浆料性能最优;固含量为68.4%～69.4%时最适合浸渍;对辊间距与前驱体浸浆量的关系紧密,较佳的d/h(其中d为对辊间距,h为海绵高度)控制范围为9.45%～10.35%。
(3)微波干燥提高了复合泡沫陶瓷的抗压强度和成品率。实验采用微波干燥方式有效地减少了椭圆变形,增加了浸浆量的限制范围,因此,泡沫陶瓷制品的抗压强度和成品率得到提高,同时提高了干燥效率,节约了能源。
(4)通过对不同配方陶瓷烧结温度的研究,分析得到烧结过程中陶瓷物相的演变,同时考察了烧结温度对陶瓷性能的影响,得出配方B为最佳配方;通过对配方B陶瓷不同烧结保温时间的研究,得到了保温时间对复合泡沫陶瓷性能的影响,实验确定复合陶瓷较佳的烧结温度为1500℃,保温时间为90min,该工艺条件制备的复合泡沫陶瓷开孔率达到81.2%,抗压强度达到1.21MPa,抗热震性能(D_(st))为0.52。
(5)研究发现,添加Y_2O_3、CaO不仅能有效促进氧化铝/莫来石复合泡沫陶瓷材料的烧结,提高陶瓷致密度,而且还能够显著提高复合泡沫陶瓷的抗压强度和抗热震性能。
采用上述方法所制备的复合泡沫陶瓷材料不仅能较好地解决普通泡沫陶瓷强度低,抗热震性能差的问题,而且制备成本低,绿色环保,具有较好的工业应用前景。
Ceramic foam with high porosity (70%-90%)and a structure of open cells in a three-dimensional network is a new type porous ceramics material made by special technique. It has many good performances such as good chemical stability, high intensity, high temperature resistance, good thermal shock resistance, large specific surface area, and so on. Because of the low cost and high efficacy, alumina-mullite ceramic foams has been widely concerned in the industry.
According to those disadvantages of ordinary clayey foam ceramics, such as low strength, low thermal shock resistance, and narrow scope of application, and the high production temperature and high cost of ceramic foams which have single component such as SiC, AlN and ZrO_2, We carried on the study on the preparation of alumina-mullite ceramic foams with polymer-sponge method, gave a systematic research on the effect of different factors on the performance of material. The research results are as follow:
(1) Pre-treatment of polymer foam increased the grouting-absorption capacity of polymeric sponge. Choose the polymeric sponge as the precursor of ceramic foams. Through alkali treatment, the film of polymeric sponge between stalks was destroyed, and the roughness of the polymeric sponge surface roughness can be increased. And then with CMC modification added, the wetting ability and grouting-absorption capacity of polymeric sponge were increased.
(2) Through adding appropriate dispersant, we can obtain the slurry with high solid content, good equality and stabilization, and excellent rheology. It was found that the best aqueous slurry can be obtained by adding 0.4% quality content PMAA-NH_4. And the slurry was most suitable for the impregnation when solid content was between 68.4%-69.4%. The gap of two-parallel rolls has a closed relationship with the grouting-absorption capacity of precursor. The best d/h(d- the distance of the gap of two-parallel rolls, h-height of polymeric sponge) was 9.45%-10.35%.
(3) The compressive strength and yield of complex ceramic foams was increased by microwave drying method. By microwave drying method, elliptical deformation was reduced effectively and the limit of grouting-absorption capacity was enlarged. So the compressive strength and yield of ceramic foams was increased. Moreover it increased the drying efficiency, and saved the energy.
(4) According to the research on the sintering temperature of ceramic with different recipe, the evolution of ceramic phase was studied. Through observing the effect of sintering temperature on ceramic performance, the best recipe B was finally confirmed. By studying on different sinter-holding time with recipe B, the influence of holding time on ceramic foam performance was obtained. The optimum sintering temperature of alumina-mullite ceramic foam was determined as 1500℃, and the optimum holding time was 90min. Under this condition, the porosity of alumina-mullite ceramic foam product was increase to 81.2%, the compressive strength was 1.21Mpa, and the thermal shock resistance (D_(st)) was 0.52.
(5) It was found that additives Y_2O_3 and CaO had a promoting effect on the sintering and density improving of alumina-mullite ceramic foams. Moreover, they could improve the compressive strength and thermal shock resistance greatly.
Prepare composite ceramic foam with above method can not only solve the problem of low strength and thermal shock resistance, but also reduce the cost and be environmental. It has good prospect for industrial application.
引文
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