CN106673703A - 一种轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法 - Google Patents
一种轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法 Download PDFInfo
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title abstract description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title abstract 6
- 229910052726 zirconium Inorganic materials 0.000 title abstract 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 39
- 239000002002 slurry Substances 0.000 claims abstract description 25
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- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 3
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- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
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- VCRLKNZXFXIDSC-UHFFFAOYSA-N aluminum oxygen(2-) zirconium(4+) Chemical compound [O--].[O--].[Al+3].[Zr+4] VCRLKNZXFXIDSC-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，包括以下步骤：1)配制总固相含量为7～45wt％的氧化锆、氧化铝和二氧化硅溶胶的混合浆料，并进行球磨；2)将球磨好的上述浆料调节pH，加入浆料总量0.006～0.8wt％的粉体疏水化修饰剂；3)将步骤2)所得浆料进行发泡得到氧化铝和氧化锆粉体均匀混合的颗粒稳定泡沫浆料，然后在石膏板上注模，干燥；4)将步骤3)所得的干燥坯体在1300～1650℃烧结。本发明可获得最高气孔率高达98.7％的多孔氧化锆增强氧化铝陶瓷，其气孔率可以与气凝胶相媲美。该泡沫结构气孔均匀完整、以闭孔为主，导热系数最低的样导热系数为0.04W/K·m，可以作为轻质阻热材料应用于高温保温耐火领域。
Description
技术领域
本发明属于无机材料技术领域，具体涉及具有高强度、低密度、低热导率的无机多孔材料的制备方法，尤其是涉及一种轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法。
背景技术
多孔氧化物陶瓷结合了泡沫材料和氧化物陶瓷的优点，具有保温绝热性能好，密度小，耐高温、耐腐蚀、高温状态下化学稳定等许多特点。其中，氧化锆增强氧化铝陶瓷是一种综合性能优良的工程材料，在工程领域广泛应用，掺杂少量氧化物稳定的四方氧化锆陶瓷在外力作用下还具有诱导相转变而增韧的特点。更重要的是，氧化锆陶瓷的本征导热系数很低，常温下只有2W/K·m，相比于常见的氧化物陶瓷在保温性能上具有明显的优势。
随着现代工业的飞速发展，对高温耐火保温材料的阻热性能提出了更高的要求，提高多孔材料的气孔率相比于其他方法是最直接也是最廉价的方法，因此进一步降低多孔材料的导热系数一直是研究的热点。具有超高气孔率的气凝胶的出现使其成为耐火保温领域中绝热性能最好的一类产品。然而气凝胶需要超临界干燥，制备成本高昂，而且还存在机械强度低，难以制备大尺寸块材等一系列问题。
发明内容
针对上述现有技术存在的问题，本发明开发了一种具有闭孔结构的多孔陶瓷，其超高的气孔率和保温性能可以与无机气凝胶相媲美。而且其制备工艺简单，成本较低，具有很好的应用价值。本发明将致密陶瓷领域常见的氧化锆增强氧化铝陶瓷原理应用于高气孔率多孔陶瓷的制备，有效提高了其机械强度。此外，本发明将金属铸造领域中常用的二氧化硅溶胶增强型壳强度的方法应用于陶瓷直接发泡环节，有效提高了干燥陶瓷泡沫坯体的强度。
本发明采用技术方案如下，一种轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，包括以下步骤：
1)配制总固相含量为7～45wt％的氧化锆、氧化铝和二氧化硅溶胶的混合浆料，并进行球磨。
2)将球磨好的上述浆料调节pH，加入浆料总量0.006～0.8wt％的粉体疏水化修饰剂，以提高陶瓷粉体的疏水性。
3)将所得浆料进行发泡得到氧化铝和氧化锆粉体均匀混合的颗粒稳定泡沫浆料，然后在石膏板上注模，干燥,
4)将步骤3)所得的干燥坯体在1300～1650℃烧结。
进一步，步骤1)中所述浆料含有氧化锆1.8～15wt％,氧化铝5～35wt％，二氧化硅溶胶颗粒0.2～0.5wt％。所述氧化锆和氧化铝粉体粒径为50nm～5μm，所述二氧化硅溶胶颗粒粒径为15～30nm。
优选的，所述氧化锆为氧化铱稳定的四方氧化锆。
进一步，所述粉体疏水化修饰剂为癸酸、十六烷基硫酸钠、十八烷基硫酸钠、十二烷基硫酸钠中的一种。选择癸酸时，浆料的pH调节至4.5～5.5之间；选择十六烷基硫酸钠、十二烷基硫酸钠或十八硫酸钠时，浆料的pH调节至3.0～9.5之间。
进一步，步骤3)中所述发泡采用机械搅拌法，所述干燥的方法选用在石膏板上常温常压干燥、40～70℃的烘箱干燥或间歇式微波干燥。在不追求干燥效率的时候，优选在石膏板上常温常压干燥。
上述方法制备的氧化锆增强氧化铝多孔陶瓷，其气孔率为87.4～98.7％。抗压强度是相同气孔率下的氧化铝多孔陶瓷抗压强度的1.5～1.9倍。导热系数介于0.04～0.28W/K·m之间。
本发明的有益效果是：①使用本发明所用的粉体疏水化修饰剂，通过调节pH至规定值可实现同时对氧化铝和氧化铝粉体表面的疏水化改性从而制备超稳定的陶瓷颗粒泡沫浆料，无需采用凝胶等方式辅助固化，且粉体疏水化修饰剂添加量少，烧结时无需排胶工序。②创新性地将铸造领域常用的硅溶胶应用于泡沫陶瓷的成型，提高了干燥泡沫坯体的强度。③创新性地将致密陶瓷制备领域中的氧化锆增韧氧化铝原理应用在多孔陶瓷制备领域，大大提高了其机械强度。④所述多孔氧化锆增强氧化铝陶瓷密度小、导热系数低，可以作为性能优良的保温耐火材料在工程领域推广应用。⑤气孔率最高的样品在气孔率保温性能上可以与无机气凝胶媲美，同时又克服了气凝胶强度低、应用受限、难以制备大尺寸块材等问题，因而可以在部分领域作为低成本无机多孔材料取代气凝胶。⑥通过调节粉体疏水化修饰剂种类及数量、粉体固相含量、pH值、烧结温度等参数可以实现对氧化锆增韧氧化铝多孔陶瓷微观结构、气孔率、导热系数、抗压强度等性能的精确调控，可以精确产出所需性能的多孔陶瓷。⑦本发明工艺流程简单，成本低廉，可以制备较大尺寸的块材(如图1所示)，每个生产环节不产生有毒、有害物质。
附图说明
图1是本发明方法生产的轻质高强氧化锆增强氧化铝多孔陶瓷照片。
图2是本发明方法中轻质高强氧化锆增强氧化铝多孔陶瓷的干燥泡沫坯体的微观照片。
图3是本发明方法生产的轻质高强氧化锆增强氧化铝多孔陶瓷烧结后的氧化锆增强氧化铝多孔陶瓷微观照片。
具体实施方式
下面结合附图和实施例，对本发明进一步详细说明。
图1是本发明方法生产的轻质高强氧化锆增强氧化铝多孔陶瓷照片。图2是本发明方法中轻质高强氧化锆增强氧化铝多孔陶瓷的干燥泡沫坯体的微观照片。可以看到硅凝胶填充了陶瓷颗粒之间的缝隙，因此粉体在硅凝胶的胶结作用下得以均匀而又紧密的排列，使得干燥泡沫坯体的强度有效提高。图3是本发明方法生产的轻质高强氧化锆增强氧化铝多孔陶瓷烧结后的氧化锆增强氧化铝多孔陶瓷微观照片。其中白色晶粒为氧化锆，灰色晶粒为氧化铝。氧化锆粉体和氧化铝粉体在浆料中混合均匀，氧化锆晶粒均匀嵌入氧化铝晶粒中，起到增韧和钉扎的作用，因此抗压强度相比同气孔率下的多孔氧化铝陶瓷得到有效提高。
实施例1
(1)配制固相含量为4wt％氧化锆(D50＝0.6μm)、16wt％氧化铝(D50＝0.5μm)、0.3wt％的二氧化硅溶胶(D50＝20nm)的混合浆料，利用滚筒球磨机球磨4h。；
(2)在上述球磨后的浆料中加入0.05wt％的癸酸，然后用稀盐酸调节pH至5.1。
(3)利用机械搅拌机在1800rmp转速下搅拌发泡10min得到陶瓷颗粒稳定泡沫浆料，在石膏板上注模脱模并在常温常压下干燥24h。
(4)将完全干燥后的干燥泡沫坯体以5℃/min的升温速率最高加热至1400℃，保温2h。
所制备的氧化锆增强氧化铝多孔陶瓷气孔率为96.7％，抗压强度为1.12MPa，抗压强度是相同气孔率的多孔氧化铝陶瓷的1.9倍。导热系数为0.08W/K·m。
实施例2
(1)配制固相含量为9.5wt％氧化锆(D50＝0.6μm)、35wt％氧化铝(D50＝0.5μm)、0.5wt％的二氧化硅溶胶(D50＝20nm)的混合浆料，利用滚筒球磨机球磨6h。；
(2)在上述球磨后的浆料中加入0.8wt％的十六烷基硫酸钠，然后用稀盐酸调节pH至4.0。
(3)利用机械搅拌机在1600rmp转速下搅拌发泡10min得到陶瓷颗粒稳定泡沫浆料，在烘箱50℃干燥4h。
(4)将完全干燥后的干燥泡沫坯体以5℃/min的升温速率最高加热至1450℃，保温2h。
所制备的氧化锆增强氧化铝多孔陶瓷气孔率为87.4％，抗压强度为11.6MPa，抗压强度是相同气孔率的多孔氧化铝陶瓷的1.6倍。导热系数为0.28W/K·m。
实施例3
(1)配制固相含量为1.8wt％氧化锆(D50＝0.2μm)、5wt％氧化铝(D50＝0.2μm)、0.2wt％的二氧化硅溶胶(D50＝20nm)的混合浆料，利用滚筒球磨机球磨1h。；
(2)在上述球磨后的浆料中加入0.006wt％的十二烷基硫酸钠，然后用稀盐酸调节pH至5.5。
(3)利用机械搅拌机在1900rmp转速下搅拌发泡10min得到陶瓷颗粒稳定泡沫浆料，在石膏板上注模脱模并在常温常压下干燥24h。
(4)将完全干燥后的干燥泡沫坯体以5℃/min的升温速率最高加热至1350℃，保温2h。
所制备的氧化锆增强氧化铝多孔陶瓷气孔率为98.7％，抗压强度为0.02MPa，抗压强度是相同气孔率的多孔氧化铝陶瓷的1.5倍。导热系数为0.04W/K·m。
以上对本发明进行了详细说明，显然，只要实质上没有脱离本发明的发明点及效果、对本领域的技术人员来说是显而易见的变形，也均包含在本发明的保护范围之内。
Claims (8)
1.一种轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，所述方法包括以下步骤：
1)配制总固相含量为7～45wt％的氧化锆、氧化铝和二氧化硅溶胶的混合浆料，并进行球磨；
2)将球磨好的上述浆料调节pH，加入浆料总量0.006～0.8wt％的粉体疏水化修饰剂；
3)将步骤2)所得浆料进行发泡，然后在石膏板上注模，干燥；
4)将步骤3)所得的干燥坯体在1300～1650℃烧结。
2.按照权利要求1所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，步骤1)中所述浆料含有氧化锆1.8～14.5wt％,氧化铝5～30wt％，二氧化硅溶胶颗粒0.2～0.5wt％，所述氧化锆和氧化铝粉体粒径为50nm～5μm，所述二氧化硅溶胶颗粒粒径为15～30nm。
3.按照权利要求1或2所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，所述氧化锆为氧化铱稳定的四方氧化锆。
4.按照权利要求1所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，步骤2)中所述粉体疏水化修饰剂为癸酸、十六烷基硫酸钠、十八烷基硫酸钠、十二烷基硫酸钠中的一种。
5.按照权利要求4所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，所述粉体疏水化修饰剂选择癸酸时，浆料的pH调节至4.5～5.5之间；选择十六烷基硫酸钠、十二烷基硫酸钠或十八烷基硫酸钠时，浆料的pH调节至3.0～9.5之间。
6.按照权利要求1所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，步骤3)中所述发泡采用机械搅拌法，所述干燥选用在石膏板上常温常压干燥、40～70℃的烘箱干燥或间歇式微波干燥。
7.按照权利要求6所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法，其特征在于，步骤3)中所述干燥选用在石膏板上常温常压干燥。
8.按照权利要求1-7任一项所述轻质高强氧化锆增强氧化铝多孔陶瓷的制备方法制备的氧化锆增强氧化铝多孔陶瓷，其特征在于所述多孔陶瓷的气孔率为87.4～98.7％，抗压强度是相同气孔率下的氧化铝多孔陶瓷抗压强度的1.5～1.9倍，导热系数介于0.04～0.28W/K·m之间。
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Application publication date: 20170517 |