CN107445594B - 纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法 - Google Patents
纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法 Download PDFInfo
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- 229910052839 forsterite Inorganic materials 0.000 title claims abstract description 57
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000000843 powder Substances 0.000 claims abstract description 69
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 56
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 55
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011148 porous material Substances 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 27
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 21
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 21
- 235000014380 magnesium carbonate Nutrition 0.000 claims abstract description 21
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 20
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 7
- 235000012245 magnesium oxide Nutrition 0.000 claims description 53
- 239000002245 particle Substances 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims 1
- 238000003825 pressing Methods 0.000 abstract 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 13
- 238000011065 in-situ storage Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000008707 rearrangement Effects 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
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- 238000003756 stirring Methods 0.000 description 5
- 239000013081 microcrystal Substances 0.000 description 4
- 238000004134 energy conservation Methods 0.000 description 3
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- 238000001514 detection method Methods 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- -1 so that on one hand Substances 0.000 description 2
- 229910001720 Åkermanite Inorganic materials 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
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- 229910000514 dolomite Inorganic materials 0.000 description 1
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- 229910052609 olivine Inorganic materials 0.000 description 1
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Abstract
一种纳米孔径的多孔方镁石‑镁橄榄石陶瓷材料及其制备方法。其技术方案是：将菱镁矿细粉依次升温至600~800℃和800~1200℃，分别保温，得到高孔隙率的氧化镁粉体。按高孔隙率的氧化镁粉体为65~95wt%、硅溶胶为0.1~18wt%和二氧化硅微粉为0.1~22wt%，将高孔隙率的氧化镁粉体置于真空搅拌机中，在2.0kPa以下将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌，得到混合料。将混合料升温至110~220℃，保温，机压成型；干燥；然后在800~1200℃和1400~1600℃条件下分别保温，即得纳米孔径的多孔方镁石‑镁橄榄石陶瓷材料。本发明制备成本低廉，所制备的纳米孔径的多孔方镁石‑镁橄榄石陶瓷材料孔径为纳米级，具有体积密度小、导热系数低和强度高的特点。
Description
技术领域
本发明属于多孔方镁石-镁橄榄石陶瓷材料技术领域。尤其涉及一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法。
背景技术
随着社会经济的高速发展，能源与资源逐渐消耗殆尽，节能减排已经成为全球关注的热点之一。多孔陶瓷具有较低的导热系数和体积密度，是隔热耐火材料主要品种之一，对高温工业的节能降耗起着关键作用，已受到耐火材料研究者越来越多的关注。方镁石-镁橄榄石材料具有优异的高温力学性能和良好的化学稳定性，广泛用于玻璃窑、水泥窑等高温窑炉，因此，研究多孔方镁石-镁橄榄石陶瓷材料对高温工业的节能降耗具有现实意义。
目前关于多孔方镁石-镁橄榄石陶瓷材料的研究已有一定的进展，如“一种方镁石-橄榄石轻质保温耐火材料及其生产方法（CN1704384A）”专利技术，以菱镁矿粉、轻烧氧化镁粉和氧化硅粉为原料，以锯末、煤粉为造孔剂，制备的轻质方镁石-镁橄榄石耐火材料虽有其优点，但缺点是制品气孔孔径较大，且造孔剂完全燃烧后生成CO2，会造成二次污染；另如以镁橄榄石砂、镁砂和菱镁矿为原料（郑连营，王健东．玻璃窑用轻质镁橄榄石砖的研制．耐火材料，2012,49(2):129～13l），制备了镁橄榄石隔热材料，但该技术对原料的要求较高，其材料气孔孔径较大、孔径分布极不均、强度较低；又如“一种多孔镁橄榄石-镁黄长石复合陶瓷材料及其制备方法（CN201410362125.9）”专利技术，以白云石粉、硅石粉和菱镁矿粉为原料，制备了强度较高的多孔镁橄榄石-镁黄长石质陶瓷材料，但该陶瓷材料气孔的孔径较大、耐火度较低、强度较低。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种制备成本低廉的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料的制备方法，所制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料孔径为纳米级、体积密度小、导热系数低和强度高。
为实现上述目的，本发明采用的技术方案的步骤是：
步骤一、先将菱镁矿细粉以1~2℃/min的速率升温至600~800℃，保温1~4小时；再以2~3℃/min的速率升温至800~1200℃，保温1~5小时，冷却，得到高孔隙率的氧化镁粉体。
步骤二、按所述高孔隙率的氧化镁粉体为65~95wt%、硅溶胶为0.1~18wt%和二氧化硅微粉为0.1~22wt%，先将所述高孔隙率的氧化镁粉体置于真空搅拌机中，抽真空至2.0kPa以下，再将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌15~30分钟，关闭抽真空系统，得到混合料。
步骤三、将所述混合料升温至110~220℃，保温2~5h，冷却，在30~100MPa条件下机压成型；成型后的坯体于110~150℃条件下干燥12~36小时；然后以2~3℃/min的速率升温至800~1200℃，保温1~5小时；再以3~5℃/min速率升温至1400~1600℃，保温3~8小时，冷却，即得纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
所述菱镁矿细粉粒径小于0.088mm，所述菱镁矿细粉的MgO含量为42~50wt%。
所述硅溶胶的SiO2含量为30~40wt%。
所述二氧化硅微粉粒径小于0.002m，所述二氧化硅微粉的SiO2含量大于96wt%。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
本发明利用菱镁矿细粉在600~800℃条件下原位分解产生纳米级气孔，形成的氧化镁微晶在800~1200℃时发生表面扩散和蒸发-凝聚物质传输过程，使得氧化镁微晶之间产生一定的颈部链接，限制了烧结中后期的颗粒重排，得到了高孔隙率的氧化镁粉体，以它为原料会得到体积密度小和导热系数低的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本发明向高孔隙率的氧化镁粉体中引入硅溶胶，在真空条件下让硅溶胶中SiO2富集在颗粒颈部，通过高温下原位反应生成镁橄榄石颈部，阻碍氧化镁颗粒在高温烧结过程中的重排。
本发明向高孔隙率的氧化镁粉体中加入二氧化硅微粉以填充氧化镁粉体间的空隙，一方面会使会使氧化镁粉体间的气孔纳米化，提高了制品的强度，另一方面与氧化镁原位反应形成的镁橄榄石颈部连接，阻止了氧化镁颗粒在高温烧结过程中的重排，从而得到了纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本发明所制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料经检测：显气孔率为25~51%；体积密度为1.61~2.30g/cm3；平均孔径为500nm~1500nm；耐压强度为50~150 MPa；物相组成为方镁石和镁橄榄石。
因此，本发明制备成本低廉，所制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料孔径为纳米级，具有体积密度小、导热系数低和强度高的特点。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制。
为避免重复，先将本具体实施方式中的硅溶胶统一描述如下，实施例中不再赘述：
所述菱镁矿细粉的MgO含量为42~50wt%。
所述硅溶胶的SiO2含量为30~40wt%。
所述二氧化硅微粉的SiO2含量大于96wt%。
实施例1
一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法。本实施例所述制备方法的步骤是：
步骤一、先将菱镁矿细粉以1~2℃/min的速率升温至600~800℃，保温1~2小时；再以2~3℃/min的速率升温至800~1000℃，保温1~3小时，冷却，得到高孔隙率的氧化镁粉体。
步骤二、按所述高孔隙率的氧化镁粉体为65~75wt%、硅溶胶为8~18wt%和二氧化硅微粉为12~22wt%，先将所述高孔隙率的氧化镁粉体置于真空搅拌机中，抽真空至2.0kPa以下，再将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌15~30分钟，关闭抽真空系统，得到混合料。
步骤三、将所述混合料升温至110~220℃，保温2~5h，冷却，在30~60MPa条件下机压成型；成型后的坯体于110~150℃条件下干燥12~24小时；然后以2~3℃/min的速率升温至800~1000℃，保温1~3小时；再以4~5℃/min速率升温至1400~1500℃，保温3~5小时，冷却，即得纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本实施例所述菱镁矿细粉粒径小于0.088mm；所述二氧化硅微粉粒径小于0.002mm。
本实施例制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料：显气孔率为40~51%；体积密度为1.61~1.92g/cm3；平均孔径为500~1200nm；耐压强度为50~80MPa；物相组成为方镁石和镁橄榄石。
实施例2
一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法。本实施例所述制备方法的步骤是：
步骤一、先将菱镁矿细粉以1~2℃/min的速率升温至600~800℃，保温2~3小时；再以2~3℃/min的速率升温至1000~1200℃，保温1~3小时，冷却，得到高孔隙率的氧化镁粉体。
步骤二、按所述高孔隙率的氧化镁粉体为73~83wt%、硅溶胶为7~15wt%和二氧化硅微粉为4~13wt%，先将所述高孔隙率的氧化镁粉体置于真空搅拌机中，抽真空至1.5kPa以下，再将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌15~30分钟，关闭抽真空系统，得到混合料。
步骤三、将所述混合料升温至110~220℃，保温2~5h，冷却，在60~80MPa条件下机压成型；成型后的坯体于110~150℃条件下干燥16~28小时；然后以2~3℃/min的速率升温至1000~1200℃，保温1~3小时；再以4~5℃/min速率升温至1400~1500℃，保温4~7小时，冷却，即得纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本实施例所述菱镁矿细粉粒径小于0.044mm；所述氢氧化铝微粉粒径小于0.002mm。
本实施例制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料：显气孔率为35~45%；体积密度为1.78~2.06g/cm3；平均孔径为900~1500nm；耐压强度为70~100MPa；物相组成为方镁石和镁橄榄石。
实施例3
一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法。本实施例所述制备方法的步骤是：
步骤一、先将菱镁矿细粉以1~2℃/min的速率升温至600~800℃，保温2~4小时；再以2~3℃/min的速率升温至800~1000℃，保温3~5小时，冷却，得到高孔隙率的氧化镁粉体。
步骤二、按所述高孔隙率的氧化镁粉体为78~88wt%、硅溶胶为2~10wt%和二氧化硅微粉为3~12wt%，先将所述高孔隙率的氧化镁粉体置于真空搅拌机中，抽真空至0.5kPa以下，再将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌15~30分钟，关闭抽真空系统，得到混合料。
步骤三、将所述混合料升温至110~220℃，保温2~5h，冷却，在70~90MPa条件下机压成型；成型后的坯体于110~150℃条件下干燥20~32小时；然后以2~3℃/min的速率升温至800~1000℃，保温3~5小时；再以3~4℃/min速率升温至1500~1600℃，保温5~8小时，冷却，即得纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本实施例所述菱镁矿细粉粒径为0.022~0.074mm；所述二氧化硅微粉粒径小于0.001mm。
本实施例制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料：显气孔率为30~40%；体积密度为1.92~2.19g/cm3；平均孔径为700~1200nm；耐压强度为80~120MPa；物相组成为方镁石和镁橄榄石。
实施例4
一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料及其制备方法。本实施例所述制备方法的步骤是：
步骤一、先将菱镁矿细粉以1~2℃/min的速率升温至600~800℃，保温3~4小时；再以2~3℃/min的速率升温至1000~1200℃，保温3~5小时，冷却，得到高孔隙率的氧化镁粉体。
步骤二、按所述高孔隙率的氧化镁粉体为85~95wt%、硅溶胶为0.1~9wt%和二氧化硅微粉为0.1~8wt%，先将所述高孔隙率的氧化镁粉体置于真空搅拌机中，抽真空至1.0kPa以下，再将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌15~30分钟，关闭抽真空系统，得到混合料。
步骤三、将所述混合料升温至110~220℃，保温2~5h，冷却，在80~100MPa条件下机压成型；成型后的坯体于110~150℃条件下干燥24~36小时；然后以2~3℃/min的速率升温至1000~1200℃，保温3~5小时；再以3~4℃/min速率升温至1500~1600℃，保温4~8小时，冷却，即得纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本实施例所述菱镁矿细粉粒径小于0.074mm；所述二氧化硅微粉粒径小于0.001mm。
本实施例制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料：显气孔率为25~35%；体积密度为2.06~2.30g/cm3；平均孔径为500~1000nm；耐压强度为100~150MPa；物相组成为方镁石和镁橄榄石。
本具体实施方式与现有技术相比具有如下积极效果：
本具体实施方式利用菱镁矿细粉在600~800℃条件下原位分解产生纳米级气孔，形成的氧化镁微晶在800~1200℃时发生表面扩散和蒸发-凝聚物质传输过程，使得氧化镁微晶之间产生一定的颈部链接，限制了烧结中后期的颗粒重排，得到了高孔隙率的氧化镁粉体，以它为原料会得到体积密度小和导热系数低的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本具体实施方式向高孔隙率的氧化镁粉体中引入硅溶胶，在真空条件下让硅溶胶中SiO2富集在颗粒颈部，通过高温下原位反应生成镁橄榄石颈部，阻碍氧化镁颗粒在高温烧结过程中的重排。
本具体实施方式向高孔隙率的氧化镁粉体中加入二氧化硅微粉以填充氧化镁粉体间的空隙，一方面会使会使氧化镁粉体间的气孔纳米化，提高了制品的强度，另一方面与氧化镁原位反应形成的镁橄榄石颈部连接，阻止了氧化镁颗粒在高温烧结过程中的重排，从而得到了纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
本具体实施方式所制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料经检测：显气孔率为25~51%；体积密度为1.61~2.30g/cm3；平均孔径为500nm~1500nm；耐压强度为50~150 MPa；物相组成为方镁石和镁橄榄石。
因此，本具体实施方式制备成本低廉，所制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料孔径为纳米级，具有体积密度小、导热系数低和强度高的特点。
Claims (5)
1.一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料的制备方法，其特征在于所述制备方法的步骤是：
步骤一、先将菱镁矿细粉以1~2℃/min的速率升温至600~800℃，保温1~4小时；再以2~3℃/min的速率升温至800~1200℃，保温1~5小时，冷却，得到高孔隙率的氧化镁粉体；
步骤二、按所述高孔隙率的氧化镁粉体为65~95wt%、硅溶胶为0.1~18wt%和二氧化硅微粉为0.1~22wt%，先将所述高孔隙率的氧化镁粉体置于真空搅拌机中，抽真空至2.0kPa以下，再将硅溶胶和二氧化硅微粉倒入真空搅拌机中，搅拌15~30分钟，关闭抽真空系统，得到混合料；
步骤三、将所述混合料升温至110~220℃，保温2~5h，冷却，在30~100MPa条件下机压成型；成型后的坯体于110~150℃条件下干燥12~36小时；然后以2~3℃/min的速率升温至800~1200℃，保温1~5小时；再以3~5℃/min速率升温至1400~1600℃，保温3~8小时，冷却，即得纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
2.根据权利要求1所述的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料的制备方法，其特征在于所述菱镁矿细粉粒径小于0.088mm，所述菱镁矿细粉的MgO含量为42~50wt%。
3.根据权利要求1所述的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料的制备方法，其特征在于所述硅溶胶的SiO2含量为30~40wt%。
4.根据权利要求1所述的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料的制备方法，其特征在于所述二氧化硅微粉粒径小于0.002mm，所述二氧化硅微粉SiO2含量大于96wt%。
5.一种纳米孔径的多孔方镁石-镁橄榄石陶瓷材料，其特征在于所述纳米孔径的多孔方镁石-镁橄榄石陶瓷材料是根据权利要求1~4项中任一项所述纳米孔径的多孔方镁石-镁橄榄石陶瓷材料的制备方法所制备的纳米孔径的多孔方镁石-镁橄榄石陶瓷材料。
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