泡沫料浆压滤成型制备纳米孔氧化硅隔热材料
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摘要
本论文采用气相法制备的憎水氧化硅粉体、硬硅钙石晶须及石英纤维为主要原料，制备了三相泡沫料浆。泡沫料浆经抽滤浓缩、压滤成型、常压干燥，得到纳米孔氧化硅隔热材料。氧化硅粉体是经物理团聚的粒径为10-20μm的团聚颗粒组成的粉体，其中的团聚颗粒都是由纳米小颗粒组成的多孔结构。动态水热合成的硬硅钙石晶须在水基料浆中相互缠绕形成特殊的微孔球藻状结构，这种特殊结构在亲水的硬硅钙石晶须包裹憎水氧化硅粉体、形成稳定的三相泡沫过程中起到重要作用。另外，硬硅钙石晶须的团聚体与石英纤维、铝溶胶共同作用，可提高纳米孔氧化硅隔热材料的强度。
本研究的主要内容包括：水基料浆的制备、三相泡沫料浆的制备、泡沫料浆的浓缩和压滤成型、纳米孔氧化硅隔热材料的隔热性能研究等。
由硬硅钙石晶须和石英纤维、水和分散剂APAM（阴离子型聚丙烯酰胺）组成的水基料浆制备中，主要研究了APAM作为分散剂对各种物料的分散性能的影响。研究表明，加入质量百分数为0.06%的APAM时，通过快速搅拌可以制备出石英纤维/硬硅钙石晶须质量配比为0.4%/5%的均匀分散的水基料浆；而发泡剂SDBS（十二烷基苯磺酸钠）对水基料浆的分散特性没有显著影响。
由水基料浆和憎水氧化硅粉体组成的三相泡沫料浆的制备中，主要研究了SDBS/APAM复配溶液的发泡性能、SDBS/APAM复配溶液与憎水氧化硅粉体制备的三相泡沫的稳定性、水基料浆与憎水氧化硅粉体制备三相泡沫的稳定性。研究表明，APAM与SDBS的协同效应使SDBA/APAM复配溶液的发泡能力有一定程度提高。SDBS/APAM质量配比为1.2%/0.06%时的发泡能力最强。相同质量水基料浆与SDBS/APAM水溶液可以包裹的憎水氧化硅粉体的最大重量基本一致。但是，水基料浆与憎水氧化硅粉体形成的三相泡沫的稳定性明显优于SDBS/APAM水溶液与憎水氧化硅粉体形成的三相泡沫。而且随着硬硅钙石晶须加入量的增加，三相泡沫的稳定性更加提高。这主要是因为：三相泡沫中，憎水的氧化硅粉体被包裹在气泡中，亲水的硬硅钙石晶须分散在气泡周围的液膜中；亲水的硬硅钙石晶须吸附了大量液相，从而形成稳定的液膜包裹憎水氧化硅粉体的结构；硬硅钙石晶须与憎水的氧化硅粉体搭接，限制了相互之间的移动。
三相泡沫料浆真空抽滤浓缩过程中，大气泡消失，形成了细密的小气泡结构。随着泡沫料浆中固相含量的增加，料浆的表观粘度快速增加，泡沫稳定性提高。浓缩泡沫料浆在较低剪切速率下就可以实现粘度明显降低，从而大大提高料浆流动性，容易实现泡沫料浆在压滤成型模具中的完全填充。浓缩泡沫料浆压滤过程中，随着水分和气体的排出，憎水氧化硅粉体团聚颗粒之间及硬硅钙石晶须之间搭建的较大空隙逐渐变小、消失。成型密度为0.25g/cm~3的试样，试样中较大的空隙为团聚颗粒之间及硬硅钙石晶须之间的空隙，较大孔的孔径集中在100-200nm之间。成型密度达到0.35g/cm~3，较大孔的孔径集中在50-150nm之间。当成型密度达到0.45g/cm~3，试样中孔径主要集中在10nm和30nm两个峰值附近。
通过平板炉快速加热法测定了材料的隔热性能并直接测定了材料的导热系数，对材料的隔热性能进行了对比研究。研究表明，随着硬硅钙石晶须加入量的增加，材料的隔热性能降低。但是，为了提高材料的强度和耐热性能需要适度增加硬硅钙石晶须的加入量。硬硅钙石晶须加入量为氧化硅粉体重量的30%的典型试样NP0，在较低温度范围内，导热系数很小。NP0对波长为1-5μm的红外辐射具有较高的透过率。所以，该材料在高温下其辐射传热占主导地位，典型试样的导热系数指数增大。为了降低纳米孔氧化硅隔热材料中的辐射传热，可在热辐射传播的通路上放置具有大的吸收系数或散射系数的陶瓷粉体遮光剂。红外遮光剂的加入量有一个最佳范围，其隔热性能最好。石墨粉、氧化钛粉和氧化锆粉对应的最佳加入量分别为20%、25%和35%左右。
采用上述泡沫料浆压滤成型工艺，实现了纳米孔氧化硅柔性、刚性及多层隔热材料的制备。本论文还对纳米孔氧化硅多层隔热材料的隔热性能进行了初步研究。通过研究发现，铝箔和柔性石墨纸作为辐射屏蔽层材料，间隔层厚度为2mm左右时，可以得到总体隔热性能最好的纳米孔氧化硅多层隔热材料。这些不同力学性能的纳米孔氧化硅隔热材料可广泛应用于多种高效隔热领域。
Nano-porous SiO2insulation materials were made from three-phase foamedslurry by filter-pressing. The foamed slurry mainly consists of hydrophobic fumedsilica, xonotlite crystal whisker, guartz fiber and water. Certain amounts of waterand gas in the foamed slurry were eliminated before filter-pressing. And the formedsample was dried in the air. A hydrophobic fumed silica particle is a porousaggregate containing many nano particles. The diameter of the silica aggregates isabout10-20micron. Xonotlite crystal whiskers synthesized by dynamichydrothermal process overlap each other in water forming a interwoven porousstructure. Such a structure is important for the fact that xonotlite crystal whiskerencapsulates the hydrophobic fumed silica particles to form a stable three-phasefoam. Besides, the xonotlite crystal whisker, quartz fiber and alumina sol togetherenhance the nano-porous SiO2insulation materials.
The main content in the paper includes: process of water based slurry, processof three-phase foamed slurry, concentration of foamed slurry, filter-pressing ofconcentrated foamed slurry, and insulating performance of the nano-porous SiO2insulation materials. In the process of water based slurry, APAM is used as thedispersant agent. The effect of APAM on dispersion of the xonotlite crystal whiskerand quartz fiber in water was studied. The results show that with severe stirring thewater based slurry with mass ratio (xonotlite crystal whisker/quartz fiber) about0.4%/5%can disperse uniformly when the APAM content is about0.06%.Meanwhile, SDBS blister has no significant influence on dispersion of the waterbased slurry.
In the process of three-phase foamed slurry, the foaming of SDBA/APAMsolution, the stability of the three-phase foamed slurry with SDBA/APAM solutionand the hydrophobic fumed silica, and the three-phase foamed slurry with the waterbased slurry and the hydrophobic fumed silica were studied. It was found thatsynergism of APAM with SDBS can enhance forming performance of the SDBA/APAM solution. When SDBS/APAM in the solution is about1.2%/0.06%thesolution show the best foaming performance. Same weight of the water based slurryand the SDBA/APAM solution can encapsulate the same weight of the hydrophobicfumed silica. But the three-phase foamed slurry with the water based slurry and thehydrophobic fumed silica is apparently more stabile than that with the SDBA/APAMsolution and the hydrophobic fumed silica. As increasing of the xonotlite crystalwhisker in the water based slurry, the three-phase foamed slurry becomes much morestable. It can be seen that the hydrophobic silica particles are encapsulated in thebubble, and that the hydrophilic xonotlite crystal whisker is dispersed in the liquidmembrane of bubbles in the three-phase foamed slurry. The hydrophilic xonotlitecrystal whisker can adsorb a great amount of liquid to encapsulate the hydrophobicsilica particles. The hydrophilic xonotlite crystal whisker overlap with thehydrophobic silica particles, and the movement between them is restricted.
In the course of vacuum filtering, the foamed slurry is concentrated, and thelarge bubbles eliminated by replacing of the large bubbles with many fine bubbles.As increasing solid content in the three-phase foamed slurry, the apparent viscosityof the slurry increases quickly. All of these facts are helpful to improve the stabilityof the foam. At low shear rate, the apparent viscosity of the concentrated slurrydecreases remarkably. At the same time the pourability of the slurry increases, andthe slurry can easily fill the filter-pressing mould. In the course of filter-pressing,part of liquid and gas is discharged, and the large pores among the hydrophobicfumed silica and xonotlite crystal whisker transfer into small pores and disappearfinally. The pore diameters in sample of nano-pore SiO2insulation materials withthe density about0.25g/cm~3mainly are from100to200nm. The pore diameters insample with the density ofabout0.35g/cm~3mainly are from50to150nm. The porediameters in sample with the density o about0.45g/cm~3mainly are around10and30nm.
Thermal insulating performance is evaluated by quickly hot plate and thethermal conductivity is also tested. It was found that with increasing of xonotlitecrystal whisker in samples the thermal insulating performance decreases. But the xonotlite crystal whisker improves the strength of samples. In a typical sample theamount of xonotlite crystal whisker is about30wt%of the hydrophobic fumed silica.The typical sample, named NP0, has low thermal conductivity at lower temperatures.However, because of the high radiation transmittance for wavelength from1to5micron, the thermal conductivity of NP0exponentially increases when radiationplays a principal role at high temperatures. To decrease the radiation in nano-porousSiO2insulation materials, some ceramic powder with large absorption or scatteringcoefficient can be used as opacifier. The amount of the opacifier in nano-porous SiO2insulation materials should be optimized for obtaining the best insulatingperformance. The optimized amount of addition of graphite, titania and zirconia areabout20%,25%and35%, respectively.
Through filter-pressing of foamed slurry, flexible, rigid and multilayernano-porous SiO2insulation materials are fabricated. In research of nano-porousSiO2multilayer thermal insulation materials, the aluminum foil and flexible graphitepaper are used as heat screen. It was found that nano-porous SiO2multilayer thermalinsulation materials get the best thermal performance when the thickness ofnano-porous SiO2layer in the multilayer thermal insulation is about2millimeters.These nano-porous SiO2insulation materials with different mechanical property canbe used in various fields as high performance insulation materials.
本研究的主要内容包括：水基料浆的制备、三相泡沫料浆的制备、泡沫料浆的浓缩和压滤成型、纳米孔氧化硅隔热材料的隔热性能研究等。
由硬硅钙石晶须和石英纤维、水和分散剂APAM（阴离子型聚丙烯酰胺）组成的水基料浆制备中，主要研究了APAM作为分散剂对各种物料的分散性能的影响。研究表明，加入质量百分数为0.06%的APAM时，通过快速搅拌可以制备出石英纤维/硬硅钙石晶须质量配比为0.4%/5%的均匀分散的水基料浆；而发泡剂SDBS（十二烷基苯磺酸钠）对水基料浆的分散特性没有显著影响。
由水基料浆和憎水氧化硅粉体组成的三相泡沫料浆的制备中，主要研究了SDBS/APAM复配溶液的发泡性能、SDBS/APAM复配溶液与憎水氧化硅粉体制备的三相泡沫的稳定性、水基料浆与憎水氧化硅粉体制备三相泡沫的稳定性。研究表明，APAM与SDBS的协同效应使SDBA/APAM复配溶液的发泡能力有一定程度提高。SDBS/APAM质量配比为1.2%/0.06%时的发泡能力最强。相同质量水基料浆与SDBS/APAM水溶液可以包裹的憎水氧化硅粉体的最大重量基本一致。但是，水基料浆与憎水氧化硅粉体形成的三相泡沫的稳定性明显优于SDBS/APAM水溶液与憎水氧化硅粉体形成的三相泡沫。而且随着硬硅钙石晶须加入量的增加，三相泡沫的稳定性更加提高。这主要是因为：三相泡沫中，憎水的氧化硅粉体被包裹在气泡中，亲水的硬硅钙石晶须分散在气泡周围的液膜中；亲水的硬硅钙石晶须吸附了大量液相，从而形成稳定的液膜包裹憎水氧化硅粉体的结构；硬硅钙石晶须与憎水的氧化硅粉体搭接，限制了相互之间的移动。
三相泡沫料浆真空抽滤浓缩过程中，大气泡消失，形成了细密的小气泡结构。随着泡沫料浆中固相含量的增加，料浆的表观粘度快速增加，泡沫稳定性提高。浓缩泡沫料浆在较低剪切速率下就可以实现粘度明显降低，从而大大提高料浆流动性，容易实现泡沫料浆在压滤成型模具中的完全填充。浓缩泡沫料浆压滤过程中，随着水分和气体的排出，憎水氧化硅粉体团聚颗粒之间及硬硅钙石晶须之间搭建的较大空隙逐渐变小、消失。成型密度为0.25g/cm~3的试样，试样中较大的空隙为团聚颗粒之间及硬硅钙石晶须之间的空隙，较大孔的孔径集中在100-200nm之间。成型密度达到0.35g/cm~3，较大孔的孔径集中在50-150nm之间。当成型密度达到0.45g/cm~3，试样中孔径主要集中在10nm和30nm两个峰值附近。
通过平板炉快速加热法测定了材料的隔热性能并直接测定了材料的导热系数，对材料的隔热性能进行了对比研究。研究表明，随着硬硅钙石晶须加入量的增加，材料的隔热性能降低。但是，为了提高材料的强度和耐热性能需要适度增加硬硅钙石晶须的加入量。硬硅钙石晶须加入量为氧化硅粉体重量的30%的典型试样NP0，在较低温度范围内，导热系数很小。NP0对波长为1-5μm的红外辐射具有较高的透过率。所以，该材料在高温下其辐射传热占主导地位，典型试样的导热系数指数增大。为了降低纳米孔氧化硅隔热材料中的辐射传热，可在热辐射传播的通路上放置具有大的吸收系数或散射系数的陶瓷粉体遮光剂。红外遮光剂的加入量有一个最佳范围，其隔热性能最好。石墨粉、氧化钛粉和氧化锆粉对应的最佳加入量分别为20%、25%和35%左右。
采用上述泡沫料浆压滤成型工艺，实现了纳米孔氧化硅柔性、刚性及多层隔热材料的制备。本论文还对纳米孔氧化硅多层隔热材料的隔热性能进行了初步研究。通过研究发现，铝箔和柔性石墨纸作为辐射屏蔽层材料，间隔层厚度为2mm左右时，可以得到总体隔热性能最好的纳米孔氧化硅多层隔热材料。这些不同力学性能的纳米孔氧化硅隔热材料可广泛应用于多种高效隔热领域。
Nano-porous SiO2insulation materials were made from three-phase foamedslurry by filter-pressing. The foamed slurry mainly consists of hydrophobic fumedsilica, xonotlite crystal whisker, guartz fiber and water. Certain amounts of waterand gas in the foamed slurry were eliminated before filter-pressing. And the formedsample was dried in the air. A hydrophobic fumed silica particle is a porousaggregate containing many nano particles. The diameter of the silica aggregates isabout10-20micron. Xonotlite crystal whiskers synthesized by dynamichydrothermal process overlap each other in water forming a interwoven porousstructure. Such a structure is important for the fact that xonotlite crystal whiskerencapsulates the hydrophobic fumed silica particles to form a stable three-phasefoam. Besides, the xonotlite crystal whisker, quartz fiber and alumina sol togetherenhance the nano-porous SiO2insulation materials.
The main content in the paper includes: process of water based slurry, processof three-phase foamed slurry, concentration of foamed slurry, filter-pressing ofconcentrated foamed slurry, and insulating performance of the nano-porous SiO2insulation materials. In the process of water based slurry, APAM is used as thedispersant agent. The effect of APAM on dispersion of the xonotlite crystal whiskerand quartz fiber in water was studied. The results show that with severe stirring thewater based slurry with mass ratio (xonotlite crystal whisker/quartz fiber) about0.4%/5%can disperse uniformly when the APAM content is about0.06%.Meanwhile, SDBS blister has no significant influence on dispersion of the waterbased slurry.
In the process of three-phase foamed slurry, the foaming of SDBA/APAMsolution, the stability of the three-phase foamed slurry with SDBA/APAM solutionand the hydrophobic fumed silica, and the three-phase foamed slurry with the waterbased slurry and the hydrophobic fumed silica were studied. It was found thatsynergism of APAM with SDBS can enhance forming performance of the SDBA/APAM solution. When SDBS/APAM in the solution is about1.2%/0.06%thesolution show the best foaming performance. Same weight of the water based slurryand the SDBA/APAM solution can encapsulate the same weight of the hydrophobicfumed silica. But the three-phase foamed slurry with the water based slurry and thehydrophobic fumed silica is apparently more stabile than that with the SDBA/APAMsolution and the hydrophobic fumed silica. As increasing of the xonotlite crystalwhisker in the water based slurry, the three-phase foamed slurry becomes much morestable. It can be seen that the hydrophobic silica particles are encapsulated in thebubble, and that the hydrophilic xonotlite crystal whisker is dispersed in the liquidmembrane of bubbles in the three-phase foamed slurry. The hydrophilic xonotlitecrystal whisker can adsorb a great amount of liquid to encapsulate the hydrophobicsilica particles. The hydrophilic xonotlite crystal whisker overlap with thehydrophobic silica particles, and the movement between them is restricted.
In the course of vacuum filtering, the foamed slurry is concentrated, and thelarge bubbles eliminated by replacing of the large bubbles with many fine bubbles.As increasing solid content in the three-phase foamed slurry, the apparent viscosityof the slurry increases quickly. All of these facts are helpful to improve the stabilityof the foam. At low shear rate, the apparent viscosity of the concentrated slurrydecreases remarkably. At the same time the pourability of the slurry increases, andthe slurry can easily fill the filter-pressing mould. In the course of filter-pressing,part of liquid and gas is discharged, and the large pores among the hydrophobicfumed silica and xonotlite crystal whisker transfer into small pores and disappearfinally. The pore diameters in sample of nano-pore SiO2insulation materials withthe density about0.25g/cm~3mainly are from100to200nm. The pore diameters insample with the density ofabout0.35g/cm~3mainly are from50to150nm. The porediameters in sample with the density o about0.45g/cm~3mainly are around10and30nm.
Thermal insulating performance is evaluated by quickly hot plate and thethermal conductivity is also tested. It was found that with increasing of xonotlitecrystal whisker in samples the thermal insulating performance decreases. But the xonotlite crystal whisker improves the strength of samples. In a typical sample theamount of xonotlite crystal whisker is about30wt%of the hydrophobic fumed silica.The typical sample, named NP0, has low thermal conductivity at lower temperatures.However, because of the high radiation transmittance for wavelength from1to5micron, the thermal conductivity of NP0exponentially increases when radiationplays a principal role at high temperatures. To decrease the radiation in nano-porousSiO2insulation materials, some ceramic powder with large absorption or scatteringcoefficient can be used as opacifier. The amount of the opacifier in nano-porous SiO2insulation materials should be optimized for obtaining the best insulatingperformance. The optimized amount of addition of graphite, titania and zirconia areabout20%,25%and35%, respectively.
Through filter-pressing of foamed slurry, flexible, rigid and multilayernano-porous SiO2insulation materials are fabricated. In research of nano-porousSiO2multilayer thermal insulation materials, the aluminum foil and flexible graphitepaper are used as heat screen. It was found that nano-porous SiO2multilayer thermalinsulation materials get the best thermal performance when the thickness ofnano-porous SiO2layer in the multilayer thermal insulation is about2millimeters.These nano-porous SiO2insulation materials with different mechanical property canbe used in various fields as high performance insulation materials.
引文
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