太阳能潜—显热储热复相陶瓷的研究
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摘要
太阳能具有资源丰富、取之不尽、用之不竭、不会污染环境和破坏生态平衡等优点。太阳能热发电是最可能引起能源革命、实现大功率发电、替代常规能源的最经济手段之一。但是太阳能具有间歇性和不稳定性的特点,必须使用蓄热材料来提高太阳能的利用率及降低使用成本。而显热储热材料存在储热密度和储热效率低等不足之处,单一的相变材料在使用时会发生固态-液态间的相互转化,必须使用专门的容器加以封装,这不但会增加传热介质与相变材料之间的热阻,提高热损耗降低传热效率,而且易发生过冷、相分离、老化和容器腐蚀等问题,特别是高温相变材料,热损耗和容器腐蚀问题极其严重,大大增加了固-液相变材料的使用成本。
基于单一的显热或潜热储热材料的不足,本文研究制备了太阳能潜热-显热复合储热陶瓷材料,研究了不同的配方组成和烧成温度对Al2O3-ZrO2(AZ系)和Al2O3-SiC-ZrO2(ASZ系)两个系列复合陶瓷材料的结构、性能的影响,研究了相变材料的性能,研究了封装剂的配方组成、成型方式、烧成制度及其与基体材料的结合机理,设计了相变材料在蜂窝陶瓷基体中不同的填充方式和填充量,计算了材料相应的潜-显热储热密度。
以α-Al203、部分稳定氧化锆(PSZ)(Y2O35.2%)、红柱石、高岭土、堇青石、桂广滑石为主要原料,设计了AZ系列配方组成,干法球磨、半干压成型,采用无压烧结法制备AZ系复合陶瓷材料。利用XRD、SEM等测试手段对AZ系配方样品进行了性能和微观结构测试。结果表明,微米级部分稳定氧化锆的加入会显著提高样品的机械强度,堇青石的加入会显著提高样品的抗热震性能,加入20wt%的微米级氧化锆比加入10wt%的微米级氧化锆更有利于提高样品的机械强度,加入20wt%的堇青石比加入10wt%的堇青石更有利于提高样品的抗热震性能。当微米氧化锆和堇青石添加量各为10wt%时,在1340℃烧成温度下保温2h可制备出性能优良的AZ系蓄热陶瓷基体材料(B4配方),这种材料的气孔率为31.48%、吸水率为12.59%、体积密度为2.50g·cm-3、抗折强度为60.83MPa、热震(室温～800℃,气冷)30次不开裂,且热震后抗折强度为68.83MPa(强度增长率为13.15%),样品的热膨胀系数为5.26×10-6℃-1,且在600℃时,比热容为0.28kJ·(kg·K)-1、导温系数为0.01cm2·s-1、导热系数为0.45W·(m·K)-1蓄热密度为240.42kJ·kg-1。相组成分析表明样品主晶相为刚玉、四方氧化锆、红柱石、莫来石、堇青石。SEM研究结果表明,B4配方样品热震前后均较致密,少量连通气孔,气孔尺寸为零点几μm～50μm,晶粒之间生长发育良好,晶粒尺寸为10μm～80μm,被少量玻璃相包裹紧密连接,球状的氧化锆晶体与氧化铝晶体呈晶间型紧密连接,赋予了样品较高的强度和抗热震性。可作为太阳能热发电用蓄热材料的基体材料。
以α-Al2O3、PSZ(Y2O35.2%)、碳化硅、红柱石、堇青石、桂广滑石为主要原料,设计了ASZ系列配方组成,干法球磨、半干压成型,采用无压烧结法制备ASZ系复合陶瓷材料。利用XRD、SEM等测试手段对ASZ系配方样品进行了性能和微观结构测试。结果表明,随着碳化硅含量的增加,样品的机械强度逐渐增加,抗热震性能也有所改善；当碳化硅添加量为50wt%时,在1280℃烧成温度下保温2h可制备出性能优良的ASZ系蓄热陶瓷基体材料(C5配方),这种材料的气孔率为24.88%、吸水率为10.44%、体积密度为2.38g·cm-3、抗折强度为66.20MPa、热震(室温～800℃,气冷)30次不开裂,且热震后抗折强度为76.99MPa(强度增长率为27.89%),样品的热膨胀系数为5.85×10-6℃-1,且在600℃时,比热容为1.05kJ·(kg·K)-1、导温系数为0.01cm2·s-1、导热系数为2.26W·(m·K)-1、蓄热密度为916.91kJ·kg-1。相组成分析表明样品主晶相为刚玉、碳化硅、硅酸锆、莫来石、堇青石。SEM研究结果表明,C5配方样品热震前后均较致密,少量连通气孔,气孔尺寸为零点几μm～50μm,晶粒之间生长发育良好,晶粒尺寸为10μm～80μm,被少量玻璃相包裹紧密连接,球状的氧化锆晶体与氧化铝晶体呈晶间型紧密连接,赋予了样品较高的强度和抗热震性。满足太阳能热发电用蓄热材料的基体材料要求。
以C5配方为主要原料,加入不同量的高温粘结剂A,设计了封装剂配方组成,采用塑压成型和两段式烧成技术制备样品。利用测试样品抗热震性和SEM显微结构研究分析了封装剂与基体材料的结合性。结果表明：加入30wt%高温粘结剂A的封装剂与基体材料结合性良好,其它5组配方样品均出现不同程度的开裂或分层现象。计算了相变材料在蜂窝陶瓷中填充在不同位置和不同含量后的材料的储热密度,结果表明,随着相变材料封装量的增加,潜热-显热复合陶瓷的储热密度增加；随着温度的升高,储热密度也随着提高。当相变材料填充了蜂窝陶瓷的2/3孔洞及每个孔洞填充2/3容积时,温度为600℃时,最佳配方C5样品的储热密度为1132.16kJ·kg-1,温度升至1000℃时,最佳配方C5样品的储热密度为1590.80 kJ·kg-1。研究结果表明,ASZ陶瓷封装PCM的潜热-显热复相陶瓷储热密度显著高于单一的显热或潜热储热密度,是一种优良的太阳能高温储热材料。
Solar energy has a rich, inexhaustible, and will not pollute the environment and damage the ecological balance and so on. Solar thermal power generation is one of the most economic ways which is the most likely to cause an energy revolution, to achieve high power generation, alternative to conventional energy sources. However, solar energy has intermittent and instability characteristics, so the heat storage material must be used to improve the utilization of solar energy to reduce the cost. The heat storage material has low heat storage density and thermal storage efficiency and so on, a single phase change materials will occur in the use of solid-liquid inter-conversion, must be packaged by a special container, which will not only increase the transfer thermal medium and the thermal resistance between the phase change material, improve heat transfer efficiency and reduce heat loss, but also can prone to cold, phase separation, aging, and container corrosion problems, particularly the high temperature phase change materials, heat loss and the container corrosion problems is extremely seriously, and increasing the use cost of the solid-liquid phase change materials.
Based on the defeat of single sensible heat or latent heat storage materials, solar latent-heat storage composite ceramics were prepared in this paper, the effect of structure, properties by the different formulations and firing temperature of Al2O3-ZrO2 (AZ series) and Al2O3-SiC-ZrO2 (ASZ series) two series of composite ceramic material, the performance of phase change material, the formulations, molding methods, firing system and the combination of mechanism of packing agent were studied, the phase change material in the honeycomb ceramic in different fill ways and quantities were designed and the latent-heat storage density of materials were calculated.
Using theα-Al2O3, partially stabilized zirconia(PSZ)(Y2O3 5.2%), andalusite, kaolin, cordierite, talc as the main raw material, AZ series formula composition were designed, dry milling, semi-dry press molding, and the composite ceramic materials of AZ series were prepared by pressureless sintering method. The performance and microstructure of the samples were tested by XRD, SEM and other means. The results show that the mechanical strength of the samples were significantly improved by the addition of micro-level partially stabilized zirconia, the thermal shock resistance of the samples were significantly improved by the addition of cordierite, the mechanical strength of the samples were improved by adding 20wt% than 10wt% of the micro-level zirconia, the thermal shock resistance of the samples were improved by adding 20wt% than 10wt% of cordierite. When the addition of micron zirconia and cordierite is 10wt%, the thermal storage ceramic matrix material of AZ series (B4 formula) were prepared by fired at 1340℃for 2h, the porosity was 31.48%, the water absorption was 12.59%, the bulk density was 2.50g·cm-3, the bending strength was 60.83MPa, the sample wasn't cracked by thermal shock resistance (room temperature-800℃, air-cooled) after 30 times, and flexural strength after thermal shock was 68.83 MPa (the growth rate of strength was 13.15%), the thermal expansion coefficient of the sample was 5.26×10-6℃-1, and the heat capacity was 0.28kJ·(kg·K)-1, the thermal conductivity coefficient was 0.01cm2·s-1, the thermal conductivity was 0.45 W·m·K)-1, the heat storage density was 240.42kJ·kg-1 at 600℃. XRD analysis showed that the main phase of the corundum samples were tetragonal zirconia, andalusite, mullite, cordierite. SEM results showed that the sample was dense of B4 formula before and after thermal shock, a small vent hole and the size were a few tenths ofμm-50μm, the grains were growth and development good, the grain size was 10μm-80μm, and were packaged by a small amount of glass phase and connected closely, spherical alumina zirconia crystal and the crystal was closely connected by the way of intergranular type, which can get the high intensity and thermal shock resistance of the samples. Which can be used as the heat storage matrix material of solar thermal power generation.
Using theα-Al2O3, PSZ(Y2O35.2%), silicon carbide, andalusite, cordierite, talc as the main raw material, ASZ series formula composition were designed, dry milling, semi-dry press molding, and the composite ceramic materials of ASZ series were prepared by pressureless sintering method. The performance and microstructure of the samples were tested by XRD, SEM and other means. The results showed that with the increase of SiC content, the mechanical strength was increased gradually, the thermal shock resistance of the samples was improved; when the addition of SiC was 50wt%, the thermal storage ceramic matrix material of ASZ series (C5 formula) were prepared by fired at 1280℃for 2h, the porosity was 24.88%, water absorption was 10.44%, bulk density was 2.38g·cm-3, the bending strength was 66.20MPa, the sample wasn't cracked by thermal shock resistance (room temperature-800℃, air-cooled) after 30 times, and flexural strength after thermal shock was 76.99MPa (the growth rate of strength was 27.89%), the thermal expansion coefficient of the sample was 5.85×10-6℃-1, and the heat capacity was 1.05kJ·(kg·K)-1, the thermal conductivity coefficient was 0.01cm2·s-1, the thermal conductivity was 2.26W·(m·K)-1, the heat storage density was 916.91 kJ·kg-1 at 600℃. XRD analysis showed that the main phase of the corundum samples were tetragonal zirconia, andalusite, mullite, cordierite. SEM results showed that the sample was dense of B4 formula before and after thermal shock, a small vent hole and the size were a few tenths ofμm～50μm, the grains were growth and development good, the grain size was 10μm～80μm, and were packaged by a small amount of glass phase and connected closely, spherical alumina zirconia crystal and the crystal was closely connected by the way of intergranular type, which can get the high intensity and thermal shock resistance of the samples. Which was met the requirements of heat storage matrix material of solar thermal power generation.
Using C5 formula as the main raw material, adding different amounts of high-temperature adhesives, designed formula composition of package agent, the samples were prepared by use of plastic molding and two-stage firing technology. The combination of the matrix material and the package agent were studied by using thermal shock test and SEM microstructure of the samples. The results showed that: the binding property of the package agent and matrix material is good when the high temperature binder was 30wt% of the package agent, the other 5 groups of formula samples were cracked or Stratified with varying degrees. The thermal storage density was calculated when filled in the honeycomb ceramics in different locations and filled different content of the phase change material, the results showed that with the increase of the amount of phase change materials packaged, the heat storage density of latent heat-heat ceramic composites were increased; with the increase of the temperature, the heat storage density were also increased. When the phase change material were filled with 2/3 of ceramic honeycomb holes and filled with 2/3 volume of each hole, the temperature was 600℃, the heat storage density was 1132.16kJ·kg-1 of the best formula C5, when the temperature was 1000℃, the heat storage density was 1590.80 kJ·kg-1 of the best formula C5. The results showed that the heat storage density of latent-sensible heat thermal energy storage composite ceramics which the PCM was packaged in the ASZ ceramic was significantly higher than that of a single sensible heat or latent heat storage, which is an excellent of solar high-temperature thermal storage material.
基于单一的显热或潜热储热材料的不足,本文研究制备了太阳能潜热-显热复合储热陶瓷材料,研究了不同的配方组成和烧成温度对Al2O3-ZrO2(AZ系)和Al2O3-SiC-ZrO2(ASZ系)两个系列复合陶瓷材料的结构、性能的影响,研究了相变材料的性能,研究了封装剂的配方组成、成型方式、烧成制度及其与基体材料的结合机理,设计了相变材料在蜂窝陶瓷基体中不同的填充方式和填充量,计算了材料相应的潜-显热储热密度。
以α-Al203、部分稳定氧化锆(PSZ)(Y2O35.2%)、红柱石、高岭土、堇青石、桂广滑石为主要原料,设计了AZ系列配方组成,干法球磨、半干压成型,采用无压烧结法制备AZ系复合陶瓷材料。利用XRD、SEM等测试手段对AZ系配方样品进行了性能和微观结构测试。结果表明,微米级部分稳定氧化锆的加入会显著提高样品的机械强度,堇青石的加入会显著提高样品的抗热震性能,加入20wt%的微米级氧化锆比加入10wt%的微米级氧化锆更有利于提高样品的机械强度,加入20wt%的堇青石比加入10wt%的堇青石更有利于提高样品的抗热震性能。当微米氧化锆和堇青石添加量各为10wt%时,在1340℃烧成温度下保温2h可制备出性能优良的AZ系蓄热陶瓷基体材料(B4配方),这种材料的气孔率为31.48%、吸水率为12.59%、体积密度为2.50g·cm-3、抗折强度为60.83MPa、热震(室温～800℃,气冷)30次不开裂,且热震后抗折强度为68.83MPa(强度增长率为13.15%),样品的热膨胀系数为5.26×10-6℃-1,且在600℃时,比热容为0.28kJ·(kg·K)-1、导温系数为0.01cm2·s-1、导热系数为0.45W·(m·K)-1蓄热密度为240.42kJ·kg-1。相组成分析表明样品主晶相为刚玉、四方氧化锆、红柱石、莫来石、堇青石。SEM研究结果表明,B4配方样品热震前后均较致密,少量连通气孔,气孔尺寸为零点几μm～50μm,晶粒之间生长发育良好,晶粒尺寸为10μm～80μm,被少量玻璃相包裹紧密连接,球状的氧化锆晶体与氧化铝晶体呈晶间型紧密连接,赋予了样品较高的强度和抗热震性。可作为太阳能热发电用蓄热材料的基体材料。
以α-Al2O3、PSZ(Y2O35.2%)、碳化硅、红柱石、堇青石、桂广滑石为主要原料,设计了ASZ系列配方组成,干法球磨、半干压成型,采用无压烧结法制备ASZ系复合陶瓷材料。利用XRD、SEM等测试手段对ASZ系配方样品进行了性能和微观结构测试。结果表明,随着碳化硅含量的增加,样品的机械强度逐渐增加,抗热震性能也有所改善；当碳化硅添加量为50wt%时,在1280℃烧成温度下保温2h可制备出性能优良的ASZ系蓄热陶瓷基体材料(C5配方),这种材料的气孔率为24.88%、吸水率为10.44%、体积密度为2.38g·cm-3、抗折强度为66.20MPa、热震(室温～800℃,气冷)30次不开裂,且热震后抗折强度为76.99MPa(强度增长率为27.89%),样品的热膨胀系数为5.85×10-6℃-1,且在600℃时,比热容为1.05kJ·(kg·K)-1、导温系数为0.01cm2·s-1、导热系数为2.26W·(m·K)-1、蓄热密度为916.91kJ·kg-1。相组成分析表明样品主晶相为刚玉、碳化硅、硅酸锆、莫来石、堇青石。SEM研究结果表明,C5配方样品热震前后均较致密,少量连通气孔,气孔尺寸为零点几μm～50μm,晶粒之间生长发育良好,晶粒尺寸为10μm～80μm,被少量玻璃相包裹紧密连接,球状的氧化锆晶体与氧化铝晶体呈晶间型紧密连接,赋予了样品较高的强度和抗热震性。满足太阳能热发电用蓄热材料的基体材料要求。
以C5配方为主要原料,加入不同量的高温粘结剂A,设计了封装剂配方组成,采用塑压成型和两段式烧成技术制备样品。利用测试样品抗热震性和SEM显微结构研究分析了封装剂与基体材料的结合性。结果表明：加入30wt%高温粘结剂A的封装剂与基体材料结合性良好,其它5组配方样品均出现不同程度的开裂或分层现象。计算了相变材料在蜂窝陶瓷中填充在不同位置和不同含量后的材料的储热密度,结果表明,随着相变材料封装量的增加,潜热-显热复合陶瓷的储热密度增加；随着温度的升高,储热密度也随着提高。当相变材料填充了蜂窝陶瓷的2/3孔洞及每个孔洞填充2/3容积时,温度为600℃时,最佳配方C5样品的储热密度为1132.16kJ·kg-1,温度升至1000℃时,最佳配方C5样品的储热密度为1590.80 kJ·kg-1。研究结果表明,ASZ陶瓷封装PCM的潜热-显热复相陶瓷储热密度显著高于单一的显热或潜热储热密度,是一种优良的太阳能高温储热材料。
Solar energy has a rich, inexhaustible, and will not pollute the environment and damage the ecological balance and so on. Solar thermal power generation is one of the most economic ways which is the most likely to cause an energy revolution, to achieve high power generation, alternative to conventional energy sources. However, solar energy has intermittent and instability characteristics, so the heat storage material must be used to improve the utilization of solar energy to reduce the cost. The heat storage material has low heat storage density and thermal storage efficiency and so on, a single phase change materials will occur in the use of solid-liquid inter-conversion, must be packaged by a special container, which will not only increase the transfer thermal medium and the thermal resistance between the phase change material, improve heat transfer efficiency and reduce heat loss, but also can prone to cold, phase separation, aging, and container corrosion problems, particularly the high temperature phase change materials, heat loss and the container corrosion problems is extremely seriously, and increasing the use cost of the solid-liquid phase change materials.
Based on the defeat of single sensible heat or latent heat storage materials, solar latent-heat storage composite ceramics were prepared in this paper, the effect of structure, properties by the different formulations and firing temperature of Al2O3-ZrO2 (AZ series) and Al2O3-SiC-ZrO2 (ASZ series) two series of composite ceramic material, the performance of phase change material, the formulations, molding methods, firing system and the combination of mechanism of packing agent were studied, the phase change material in the honeycomb ceramic in different fill ways and quantities were designed and the latent-heat storage density of materials were calculated.
Using theα-Al2O3, partially stabilized zirconia(PSZ)(Y2O3 5.2%), andalusite, kaolin, cordierite, talc as the main raw material, AZ series formula composition were designed, dry milling, semi-dry press molding, and the composite ceramic materials of AZ series were prepared by pressureless sintering method. The performance and microstructure of the samples were tested by XRD, SEM and other means. The results show that the mechanical strength of the samples were significantly improved by the addition of micro-level partially stabilized zirconia, the thermal shock resistance of the samples were significantly improved by the addition of cordierite, the mechanical strength of the samples were improved by adding 20wt% than 10wt% of the micro-level zirconia, the thermal shock resistance of the samples were improved by adding 20wt% than 10wt% of cordierite. When the addition of micron zirconia and cordierite is 10wt%, the thermal storage ceramic matrix material of AZ series (B4 formula) were prepared by fired at 1340℃for 2h, the porosity was 31.48%, the water absorption was 12.59%, the bulk density was 2.50g·cm-3, the bending strength was 60.83MPa, the sample wasn't cracked by thermal shock resistance (room temperature-800℃, air-cooled) after 30 times, and flexural strength after thermal shock was 68.83 MPa (the growth rate of strength was 13.15%), the thermal expansion coefficient of the sample was 5.26×10-6℃-1, and the heat capacity was 0.28kJ·(kg·K)-1, the thermal conductivity coefficient was 0.01cm2·s-1, the thermal conductivity was 0.45 W·m·K)-1, the heat storage density was 240.42kJ·kg-1 at 600℃. XRD analysis showed that the main phase of the corundum samples were tetragonal zirconia, andalusite, mullite, cordierite. SEM results showed that the sample was dense of B4 formula before and after thermal shock, a small vent hole and the size were a few tenths ofμm-50μm, the grains were growth and development good, the grain size was 10μm-80μm, and were packaged by a small amount of glass phase and connected closely, spherical alumina zirconia crystal and the crystal was closely connected by the way of intergranular type, which can get the high intensity and thermal shock resistance of the samples. Which can be used as the heat storage matrix material of solar thermal power generation.
Using theα-Al2O3, PSZ(Y2O35.2%), silicon carbide, andalusite, cordierite, talc as the main raw material, ASZ series formula composition were designed, dry milling, semi-dry press molding, and the composite ceramic materials of ASZ series were prepared by pressureless sintering method. The performance and microstructure of the samples were tested by XRD, SEM and other means. The results showed that with the increase of SiC content, the mechanical strength was increased gradually, the thermal shock resistance of the samples was improved; when the addition of SiC was 50wt%, the thermal storage ceramic matrix material of ASZ series (C5 formula) were prepared by fired at 1280℃for 2h, the porosity was 24.88%, water absorption was 10.44%, bulk density was 2.38g·cm-3, the bending strength was 66.20MPa, the sample wasn't cracked by thermal shock resistance (room temperature-800℃, air-cooled) after 30 times, and flexural strength after thermal shock was 76.99MPa (the growth rate of strength was 27.89%), the thermal expansion coefficient of the sample was 5.85×10-6℃-1, and the heat capacity was 1.05kJ·(kg·K)-1, the thermal conductivity coefficient was 0.01cm2·s-1, the thermal conductivity was 2.26W·(m·K)-1, the heat storage density was 916.91 kJ·kg-1 at 600℃. XRD analysis showed that the main phase of the corundum samples were tetragonal zirconia, andalusite, mullite, cordierite. SEM results showed that the sample was dense of B4 formula before and after thermal shock, a small vent hole and the size were a few tenths ofμm～50μm, the grains were growth and development good, the grain size was 10μm～80μm, and were packaged by a small amount of glass phase and connected closely, spherical alumina zirconia crystal and the crystal was closely connected by the way of intergranular type, which can get the high intensity and thermal shock resistance of the samples. Which was met the requirements of heat storage matrix material of solar thermal power generation.
Using C5 formula as the main raw material, adding different amounts of high-temperature adhesives, designed formula composition of package agent, the samples were prepared by use of plastic molding and two-stage firing technology. The combination of the matrix material and the package agent were studied by using thermal shock test and SEM microstructure of the samples. The results showed that: the binding property of the package agent and matrix material is good when the high temperature binder was 30wt% of the package agent, the other 5 groups of formula samples were cracked or Stratified with varying degrees. The thermal storage density was calculated when filled in the honeycomb ceramics in different locations and filled different content of the phase change material, the results showed that with the increase of the amount of phase change materials packaged, the heat storage density of latent heat-heat ceramic composites were increased; with the increase of the temperature, the heat storage density were also increased. When the phase change material were filled with 2/3 of ceramic honeycomb holes and filled with 2/3 volume of each hole, the temperature was 600℃, the heat storage density was 1132.16kJ·kg-1 of the best formula C5, when the temperature was 1000℃, the heat storage density was 1590.80 kJ·kg-1 of the best formula C5. The results showed that the heat storage density of latent-sensible heat thermal energy storage composite ceramics which the PCM was packaged in the ASZ ceramic was significantly higher than that of a single sensible heat or latent heat storage, which is an excellent of solar high-temperature thermal storage material.
引文
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