CN107382286A - 一种纳米孔径的多孔刚玉‑莫来石陶瓷及其制备方法 - Google Patents
一种纳米孔径的多孔刚玉‑莫来石陶瓷及其制备方法 Download PDFInfo
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- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 55
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 73
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 67
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000010792 warming Methods 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 20
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 239000010433 feldspar Substances 0.000 claims description 3
- 230000035699 permeability Effects 0.000 abstract description 7
- 238000003756 stirring Methods 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 9
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 238000011065 in-situ storage Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
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- 238000005245 sintering Methods 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种纳米孔径的多孔刚玉‑莫来石陶瓷及其制备方法。其技术方案是：将氢氧化铝细粉依次升温至280~450℃和800~1200℃，分别保温，得到高孔隙率的氧化铝粉体。按高孔隙率的氧化铝粉体为70~90wt%、硅溶胶为9~29wt%和二氧化硅微粉为1~10wt%配料，先将高孔隙率的氧化铝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加入所述真空搅拌机中，搅拌，得到混合料。将所述混合料在110~220℃保温，冷却，机压成型，干燥，然后依次升温至800~1100℃和1400~1600℃，分别保温，即得纳米孔径的多孔刚玉‑莫来石陶瓷。本发明所制制品的气孔孔径为纳米级，具有透气度低、导热系数低、体积稳定性好和强度高的特点。
Description
技术领域
本发明属于多孔刚玉-莫来石陶瓷技术领域。尤其涉及一种纳米孔径的多孔刚玉-莫来石陶瓷及其制备方法。
背景技术
刚玉-莫来石材料具有荷重软化温度高、抗热震性好和高温蠕变率低等优点，广泛用作高炉热风炉、加热炉等工业炉窑的内衬材料。由于刚玉-莫来石材料气孔率较低和导热系数高，会造成一定的炉衬散热损失，为了减少工业窑炉散热损失、增加刚玉-莫来石材料气孔率和降低刚玉-莫来石材料的导热系数，发展多孔刚玉-莫来石陶瓷作为工作窑炉保温材料迫在眉睫。
目前，关于制备多孔刚玉-莫来石陶瓷的研究有：如文献技术（曹贺辉，王刚，袁波等．泡沫注凝法制备刚玉-莫来石多孔陶瓷[J]．耐火材料，2013，47(5):334-337.）以板状刚玉粉、氧化铝微粉和硅溶胶为原料，采用泡沫注凝法制备了刚玉-莫来石多孔陶瓷，该方法制备的材料的不仅强度较低和气孔孔径大，且气孔孔径与体积稳定性差；又如文献技术（Yan W, Chen Q, Lin X, et al. Pore characteristics and phase compositions ofporous corundum-mullite ceramics prepared from kaolinite gangue and Al(OH)3with different amount of CaCO3 addition[J]. Journal of the Ceramic Society ofJapan, 2015, 123(1441):897-902.）采用原位分解成孔技术、以Al(OH)3和煤矸石为原料制备了多孔刚玉-莫来石陶瓷，但其气孔孔径较大、透气度较大和强度较低。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种纳米孔径的多孔刚玉-莫来石陶瓷的制备方法，所制备的纳米孔径的多孔刚玉-莫来石陶瓷透气度低、导热系数低、体积稳定性好和强度高。
为实现上述目的，本发明采用的技术方案的步骤是：
步骤一、将氢氧化铝细粉置于高温炉内，先以1~2℃/min的速率升温至280~450℃，保温1~4小时，再以2~2.9℃/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铝粉体。
步骤二、按所述高孔隙率的氧化铝粉体为70~90wt%、硅溶胶为9~29wt%和二氧化硅微粉为1~10wt%配料，先将所述高孔隙率的氧化铝粉体置于真空搅拌机中，抽真空至2.0kPa以下，再将所述硅溶胶和所述二氧化硅微粉倒入所述真空搅拌机中，搅拌15~30min，关闭抽真空***，得到混合料。
步骤三、将所述混合料在110~220℃条件下保温2~5h，冷却，在30~150MPa条件下机压成型，成型后的坯体在110℃条件下干燥12~36小时；然后将干燥后的坯体置于高温炉内，以2~3℃/min的速率升温至800~1100℃，保温1~4h，再以3~5℃/min的速率升温至1400~1600℃，保温3~8h，即得纳米孔径的多孔刚玉-莫来石陶瓷。
所述氢氧化铝细粉中的Al2O3含量为60~66wt%，所述氢氧化铝细粉的粒径小于88μm。
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97wt%，所述二氧化硅微粉的粒径小于2μm。
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：
本发明利用氢氧化铝细粉在280~450℃条件下分解产生纳米级气孔，形成氧化铝微晶，利用其在800~1200℃时会发生表面扩散物质传输过程，使氧化铝微晶之间产生颈部链接，限制烧结中后期的颗粒重排，得到高孔隙率的氧化铝粉体；采用高孔隙率的氧化铝粉体为主要原料降低了纳米孔径的多孔刚玉-莫来石陶瓷的体积密度。
本发明向高孔隙率的氧化铝粉体中引入硅溶胶，在真空条件下硅溶胶中的SiO2富集在氧化铝颗粒颈部，通过高温下原位反应生成具有一定体积膨胀的莫来石，阻碍纳米孔合并长大。
本发明向高孔隙率的氧化铝粉体中引入二氧化硅微粉以填充氧化铝粉体之间的空隙，一方面会使氧化铝颗粒间的气孔纳米化，提高了纳米孔径的多孔刚玉-莫来石陶瓷的强度，降低了制品的透气度和导热系数；另一方面二氧化硅微粉和硅溶胶与高孔隙率的氧化铝原位反应生成莫来石，由于莫来石生成在氧化铝颗粒的颈部，形成氧化铝颗粒颈部间的连接，阻止了氧化铝颗粒在高温烧结过程中的重排，同时增加了纳米孔径的多孔刚玉-莫来石陶瓷的强度和体积稳定性。
本发明所制备的纳米孔径的多孔刚玉-莫来石陶瓷经检测：显气孔率为25~55%；体积密度为1.38~2.30g/cm3；平均孔径为100~1000nm；耐压强度为40~125MPa；物相组成为刚玉相和莫来石相。
因此，本发明所制备的纳米孔径的多孔刚玉-莫来石陶瓷的气孔孔径为纳米级，具有透气度低、导热系数低、体积稳定性好和强度高的特点。
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物料统一描述如下，实施例中不再赘述：
所述氢氧化铝细粉的Al2O3含量为60~66wt%。
所述硅溶胶的SiO2含量为30~40wt%。
所述二氧化硅微粉中的SiO2含量大于97wt%。
实施例1
一种纳米孔径的多孔刚玉-莫来石陶瓷及其制备方法。本实施例所述制备方法的步骤：
步骤一、将氢氧化铝细粉置于高温炉内，先以1~2℃/min的速率升温至280~450℃，保温1~2小时，再以2~2.9℃/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铝粉体。
步骤二、按所述高孔隙率的氧化铝粉体为70~75wt%、硅溶胶为24~29wt%和二氧化硅微粉为1~5wt%配料，先将所述高孔隙率的氧化铝粉体置于真空搅拌机中，抽真空至2.0kPa以下，再将所述硅溶胶和所述二氧化硅微粉倒入所述真空搅拌机中，搅拌15~30min，关闭抽真空***，得到混合料。
步骤三、将所述混合料在110~220℃条件下保温2~3h，冷却，在30~60MPa条件下机压成型，成型后的坯体在110℃条件下干燥12~24小时；然后将干燥后的坯体置于高温炉内，以2~3℃/min的速率升温至800~1000℃，保温1~2h，再以4~5℃/min的速率升温至1400~1500℃，保温3~5h，即得纳米孔径的多孔刚玉-莫来石陶瓷。
本实施例所述氢氧化铝细粉粒径小于88μm；所述二氧化硅微粉粒径小于2μm。
本实施例所制备的纳米孔径的多孔刚玉-莫来石陶瓷经检测：显气孔率为35~55%；体积密度为1.38~1.99g/cm3；平均孔径为700~1000nm；耐压强度为40~95MPa。
实施例2
一种纳米孔径的多孔刚玉-莫来石陶瓷及其制备方法。本实施例所述制备方法的步骤：
步骤一、将氢氧化铝细粉置于高温炉内，先以1~2℃/min的速率升温至280~450℃，保温2~3小时，再以2~2.9℃/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铝粉体。
步骤二、按所述高孔隙率的氧化铝粉体为75~80wt%、硅溶胶为17~22wt%和二氧化硅微粉为3~8wt%配料，先将所述高孔隙率的氧化铝粉体置于真空搅拌机中，抽真空至1.7kPa以下，再将所述硅溶胶和所述二氧化硅微粉倒入所述真空搅拌机中，搅拌15~30min，关闭抽真空***，得到混合料。
步骤三、将所述混合料在110~220℃条件下保温3~4h，冷却，在60~90MPa条件下机压成型，成型后的坯体在110℃条件下干燥18~24小时；然后将干燥后的坯体置于高温炉内，以2~3℃/min的速率升温至1000~1100℃，保温2~4h，再以4~5℃/min的速率升温至1500~1600℃，保温3~5h，即得纳米孔径的多孔刚玉-莫来石陶瓷。
本实施例所述氢氧化铝细粉粒径小于44μm；所述氢氧化铝微粉粒径小于2μm。
本实施例所制备的纳米孔径的多孔刚玉-莫来石陶瓷经检测：显气孔率为32~45%；体积密度为1.68~2.08g/cm3；平均孔径为500~800nm；耐压强度为60~105MPa。
实施例3
一种纳米孔径的多孔刚玉-莫来石陶瓷及其制备方法。本实施例所述制备方法的步骤：
步骤一、将氢氧化铝细粉置于高温炉内，先以1~2℃/min的速率升温至280~450℃，保温2~4小时，再以2~2.9℃/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铝粉体。
步骤二、按所述高孔隙率的氧化铝粉体为75~85wt%、硅溶胶为10~19wt%和二氧化硅微粉为5~10wt%配料，先将所述高孔隙率的氧化铝粉体置于真空搅拌机中，抽真空至0.7kPa以下，再将所述硅溶胶和所述二氧化硅微粉倒入所述真空搅拌机中，搅拌15~30min，关闭抽真空***，得到混合料。
步骤三、将所述混合料在110~220℃条件下保温3~5h，冷却，在90~120MPa条件下机压成型，成型后的坯体在110℃条件下干燥16~30小时；然后将干燥后的坯体置于高温炉内，以2~3℃/min的速率升温至800~1000℃，保温1~2h，再以3~4℃/min的速率升温至1400~1500℃，保温5~8h，即得纳米孔径的多孔刚玉-莫来石陶瓷。
本实施例所述氢氧化铝细粉粒径为22~74μm；所述二氧化硅微粉粒径小于1μm。
本实施例所制备的纳米孔径的多孔刚玉-莫来石陶瓷经检测：显气孔率为28~40%；体积密度为1.83~2.20g/cm3；平均孔径为300~600nm；耐压强度为73~115MPa。
实施例4
一种纳米孔径的多孔刚玉-莫来石陶瓷及其制备方法。本实施例所述制备方法的步骤：
步骤一、将氢氧化铝细粉置于高温炉内，先以1~2℃/min的速率升温至280~450℃，保温3~4小时，再以2~2.9℃/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铝粉体。
步骤二、按所述高孔隙率的氧化铝粉体为85~90wt%、硅溶胶为9~14wt%和二氧化硅微粉为1~5wt%配料，先将所述高孔隙率的氧化铝粉体置于真空搅拌机中，抽真空至1.2kPa以下，再将所述硅溶胶和所述二氧化硅微粉倒入所述真空搅拌机中，搅拌15~30min，关闭抽真空***，得到混合料。
步骤三、将所述混合料在110~220℃条件下保温4~5h，冷却，在120~150MPa条件下机压成型，成型后的坯体在110℃条件下干燥24~36小时；然后将干燥后的坯体置于高温炉内，以2~3℃/min的速率升温至1000~1100℃，保温2~4h，再以3~4℃/min的速率升温至1500~1600℃，保温4~8h，即得纳米孔径的多孔刚玉-莫来石陶瓷。
本实施例所述氢氧化铝细粉粒径小于22μm；所述二氧化硅微粉粒径小于1μm。
本实施例所制备的纳米孔径的多孔刚玉-莫来石陶瓷经检测：显气孔率为25~35%；体积密度为1.99~2.30g/cm3；平均孔径为100~400nm；耐压强度为85~125MPa。
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氢氧化铝细粉在280~450℃条件下分解产生纳米级气孔，形成氧化铝微晶，利用其在800~1200℃时会发生表面扩散物质传输过程，使氧化铝微晶之间产生颈部链接，限制烧结中后期的颗粒重排，得到高孔隙率的氧化铝粉体；采用高孔隙率的氧化铝粉体为主要原料降低了纳米孔径的多孔刚玉-莫来石陶瓷的体积密度。
本具体实施方式向高孔隙率的氧化铝粉体中引入硅溶胶，在真空条件下硅溶胶中的SiO2富集在氧化铝颗粒颈部，通过高温下原位反应生成具有一定体积膨胀的莫来石，阻碍纳米孔合并长大。
本具体实施方式向高孔隙率的氧化铝粉体中引入二氧化硅微粉以填充氧化铝粉体之间的空隙，一方面会使氧化铝颗粒间的气孔纳米化，提高了纳米孔径的多孔刚玉-莫来石陶瓷的强度，降低了制品的透气度和导热系数；另一方面二氧化硅微粉和硅溶胶与高孔隙率的氧化铝原位反应生成莫来石，由于莫来石生成在氧化铝颗粒的颈部，形成氧化铝颗粒颈部间的连接，阻止了氧化铝颗粒在高温烧结过程中的重排，同时增加了纳米孔径的多孔刚玉-莫来石陶瓷的强度和体积稳定性。
本具体实施方式所制备的纳米孔径的多孔刚玉-莫来石陶瓷经检测：显气孔率为25~55%；体积密度为1.38~2.30g/cm3；平均孔径为100~1000nm；耐压强度为40~125MPa；物相组成为刚玉相和莫来石相。
因此，本具体实施方式所制备的纳米孔径的多孔刚玉-莫来石陶瓷的气孔孔径为纳米级，具有透气度低、导热系数低、体积稳定性好和强度高的特点。
Claims (5)
1.一种纳米孔径的多孔刚玉-莫来石陶瓷的制备方法，其特征在于所述制备方法的步骤是：
步骤一、将氢氧化铝细粉置于高温炉内，先以1~2℃/min的速率升温至280~450℃，保温1~4小时；再以2~2.9℃/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铝粉体；
步骤二、按所述高孔隙率的氧化铝粉体为70~90wt%、硅溶胶为9~29wt%和二氧化硅微粉为1~10wt%配料，先将所述高孔隙率的氧化铝粉体置于真空搅拌机中，抽真空至2.0kPa以下，再将所述硅溶胶和所述二氧化硅微粉倒入所述真空搅拌机中，搅拌15~30min，关闭抽真空***，得到混合料；
步骤三、将所述混合料在110~220℃条件下保温2~5h，冷却，在30~150MPa条件下机压成型，成型后的坯体在110℃条件下干燥12~36小时；然后将干燥后的坯体置于高温炉内，以2~3℃/min的速率升温至800~1100℃，保温1~4h，再以3~5℃/min的速率升温至1400~1600℃，保温3~8h，即得纳米孔径的多孔刚玉-莫来石陶瓷。
2.根据权利要求1所述的纳米孔径的多孔刚玉-莫来石陶瓷的制备方法，其特征在于所述氢氧化铝细粉中的Al2O3含量为60~66wt%，所述氢氧化铝细粉的粒径小于88μm。
3.根据权利要求1所述的纳米孔径的多孔刚玉-莫来石陶瓷的制备方法，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刚玉-莫来石陶瓷的制备方法，其特征在于所述二氧化硅微粉的SiO2含量大于97wt%，所述二氧化硅微粉的粒径小于2μm。
5.一种纳米孔径的多孔刚玉-莫来石陶瓷，其特征在于所述纳米孔径的多孔刚玉-莫来石陶瓷是根据权利要求1~4项中任一项所述的纳米孔径的多孔刚玉-莫来石陶瓷的制备方法所制备的纳米孔径的多孔刚玉-莫来石陶瓷。
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