CN111393156A - 堇青石多孔陶瓷的制备方法 - Google Patents

堇青石多孔陶瓷的制备方法 Download PDF

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CN111393156A
CN111393156A CN202010224276.3A CN202010224276A CN111393156A CN 111393156 A CN111393156 A CN 111393156A CN 202010224276 A CN202010224276 A CN 202010224276A CN 111393156 A CN111393156 A CN 111393156A
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李亮
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Abstract

本发明属于陶瓷材料技术领域，具体涉及堇青石多孔陶瓷的制备方法。本发明所要解决的技术问题是提供一种堇青石多孔陶瓷的制备方法，包括以下步骤：将石英砂粉、氧化铝微粉、97牌号电熔镁砂粉、结合剂、矿化剂和造孔剂混合均匀，加水，再混合均匀，得半干状态物料；将半干状态物料倒入模具中成型为半成品，半成品经煅烧，得堇青石多孔陶瓷；所述结合剂为铝酸盐水泥，所述矿化剂为钛白粉。本发明方法制备得到的堇青石多孔陶瓷具有良好的性能。

Description

堇青石多孔陶瓷的制备方法
技术领域
本发明属于陶瓷材料技术领域，具体涉及堇青石多孔陶瓷的制备方法。
背景技术
堇青石(2MgO.2Al2O3.5SiO2)是MgO.Al2O3.SiO2系统中的三元化合物，密度2.6～2.7g/cm3，熔点为1460℃，在1465℃时不一致熔融会产生莫来石和液相。由于堇青石晶体结构中存在较大空隙，对称性低且不紧密，当温度升高时，分子受热振动有足够的空间，故其热膨胀较小，且具有较好的抗热震稳定性和较低的热导率。此外，堇青石还具有耐火度高、介电常数低、化学稳定性好、介电损耗小等优良特性，在现代技术中具有重要意义。堇青石被广泛应用于汽车行业中作为催化剂载体、耐火材料中作为快速循环炉的炉衬材料，以及用于金属涂层、热交换器、微电子基板、膜支撑件和燃气燃烧器等方面。
多孔陶瓷是一种在高温下烧制得到且具有大量相互连通或闭气孔的陶瓷材料，其具有体积密度低、渗透率高、隔热性能好、寿命长、抗腐蚀、耐高温和易生成的特点。堇青石多孔陶瓷不仅具有堇青石热膨胀系数低、化学稳定性好、耐腐蚀的特点，还具备多孔陶瓷隔热性好、耐高温、低体积密度、高渗透率等性能，广泛应用于高温过滤材料、催化剂载体材料和绝缘材料等，研究堇青石多孔陶瓷的制备方法具有重要的意义。
发明内容
本发明所要解决的技术问题是提供一种堇青石多孔陶瓷的制备方法。该制备方法包括以下步骤：将石英砂粉、氧化铝微粉、97牌号电熔镁砂粉、结合剂、矿化剂和造孔剂混合均匀，加水，再混合均匀，得半干状态物料；将半干状态物料倒入模具中成型为半成品，半成品经煅烧，得堇青石多孔陶瓷；所述结合剂为铝酸盐水泥，所述矿化剂为钛白粉。
其中，上述堇青石多孔陶瓷的制备方法中，所述造孔剂为碳化硅、淀粉、石墨粉、木屑或植物纤维中的至少一种。
其中，上述堇青石多孔陶瓷的制备方法中，所述石英砂粉中SiO2≥98％。
其中，上述堇青石多孔陶瓷的制备方法中，所述氧化铝微粉中Al2O3≥99％。
其中，上述堇青石多孔陶瓷的制备方法中，所述97牌号电熔镁砂粉中MgO≥97％。
其中，上述堇青石多孔陶瓷的制备方法中，所述石英砂粉的粒度≤0.088mm。
其中，上述堇青石多孔陶瓷的制备方法中，所述97牌号电熔镁砂粉的粒度≤0.088mm。
其中，上述堇青石多孔陶瓷的制备方法中，所述碳化硅的粒度≤0.088mm。
其中，上述堇青石多孔陶瓷的制备方法中，各原料含水量在2％以下。
其中，上述堇青石多孔陶瓷的制备方法中，所述铝酸盐水泥的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的4～6％。
其中，上述堇青石多孔陶瓷的制备方法中，所述造孔剂的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的4～7％。
其中，上述堇青石多孔陶瓷的制备方法中，所述钛白粉的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的4～7％。
其中，上述堇青石多孔陶瓷的制备方法中，所述水的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的6～9％。
其中，上述堇青石多孔陶瓷的制备方法中，所述成型的压力为15～25MPa，保压5～10s。
其中，上述堇青石多孔陶瓷的制备方法中，所述煅烧的温度为1250～1350℃，时间为5～10h。
优选的，上述堇青石多孔陶瓷的制备方法中，所述煅烧的温度和时间为1300℃×8h。
本发明选用优质原料97牌号电熔镁砂、石英砂、氧化铝可以减少杂质的带入量，提高堇青石多孔陶瓷的烧结效果，对提高堇青石多孔陶瓷的抗弯强度有利；通过选择钛白粉作矿化剂，钛白粉具有较好的矿化效果，可以降低堇青石多孔陶瓷的烧结温度，同时可以进一步提高堇青石多孔陶瓷的抗弯强度；选择铝酸盐水泥作结合剂，铝酸盐水泥具有水化特性，可以提高出模样品的强度，提高半成品合格率，铝酸盐水泥中含有少量氧化钙可以起到矿化剂作用，可以在一定程度上降低堇青石多孔陶瓷烧结温度，提高堇青石多孔陶瓷的抗弯强度；造孔剂的选择主要考虑生产成本。
具体实施方式
1、检测水分
分析检测所用原料的含水量，水分含量过多，会造成混合过程中结块、粘结现象，对于水分含量超过2％，应对原料进行烘干处理，保证混合的均匀性。
2、配料
根据堇青石化学式Mg2Al4Si5O18，算出理论需要量SiO251.4％、Al2O334.9％、MgO13.7％，再以选择的原料所含SiO2、Al2O3、MgO来称量来进行配料，称取满足堇青石化学式所需要的石英砂粉、氧化铝微粉和97牌号电熔镁砂粉，并额外添加结合剂、矿化剂和造孔剂。电熔镁砂、石英砂和碳化硅粒度较大时，采用球磨机将电熔镁砂、石英砂和碳化硅磨细。
3、混合
将称量好的石英砂粉、氧化铝微粉、97牌号电熔镁砂粉、结合剂、造孔剂和矿化剂，送至强制混合机混合，将粉料混合均匀后，再添加水混合成具有一定成型性能的半干状物料。
4、成型
采用液压机将半干状态物料成型为具有一定形状的半成品。
5、烧成
半成品经过高温煅烧，得到堇青石多孔陶瓷产品。
试验例1结合剂筛选试验
以铝酸盐水泥、水玻璃分别作为结合剂进行试验，考察结合剂对抗弯强度的影响，试验结果见表1。
表1添加结合剂筛选试验
1#配方 2#配方
原料名称 配比/％ 配比/％
石英砂粉 49 49
氧化铝微粉 36 36
97牌号电熔镁砂粉 15 15
铝酸盐水泥(外加) 4
水玻璃(外加) 4
碳化硅粉(外加) 5 5
水(外加) 6 6
抗弯强度(MPa) 3.5 3
从表1可以看出，添加铝酸盐水泥作结合剂，抗弯强度较添加水玻璃高，选择铝酸盐水泥作结合剂。
试验例2矿化剂筛选试验
以钛白粉、二氧化锆分别作为矿化剂进行试验，考察矿化剂对抗弯强度的影响，试验结果见表2。
表2添加矿化剂筛选试验
3#配方 4#配方
原料名称 配比/％ 配比/％
石英砂粉 49 49
氧化铝微粉 36 36
97牌号电熔镁砂粉 15 15
铝酸盐水泥(外加) 4 4
碳化硅粉(外加) 5 5
钛白粉(外加) 6
二氧化锆(外加) 6
水(外加) 6 6
抗弯强度(MPa) 5 3.5
从表2可以看出，添加钛白粉的抗弯强度比添加二氧化锆增加得多，选择钛白粉作为矿化剂。
试验例3造孔剂筛选试验
以碳化硅粉、淀粉、石墨粉、木屑分别作为造孔剂进行试验，考察造孔剂对显气孔率的影响，试验结果见表3。
表3添加造孔剂筛选试验
5#配方 6#配方 7#配方 8#配方
原料名称 配比/％ 配比/％ 配比/％ 配比/％
石英砂粉 49 49 49 49
氧化铝微粉 36 36 36 36
97牌号电熔镁砂粉 15 15 15 15
铝酸盐水泥(外加) 4 4 4 4
钛白粉(外加) 6 6 6 6
碳化硅粉(外加) 5
淀粉(外加) 4
石墨粉(外加) 4
木屑(外加) 4
水(外加) 6 6 6 6
显气孔率/％ 31 32 33 34
从表3可以看出，添加不同的造孔剂显气孔率在31％-34％。根据多孔陶瓷通用技术条件(GBT16533-1996)标准中的要求，要求显气孔率≥30％。添加的碳化硅、淀粉、石墨粉和木屑均能达到多孔陶瓷标准中显气孔率的要求，考虑到木屑的生产成本最低，可以优先选择木屑作为造孔剂。
实施例1
(1)磨料和配料
先采用球磨机分别将97电熔镁砂、石英砂磨制成粒度≤0.088mm，再将磨细后97电熔镁砂、磨细后石英砂粉、氧化铝微粉、铝酸盐水泥、钛白粉和木屑按表4配方准确称量。
(2)混合
采用强制搅拌机先将称量好的物料干混5-8分钟，再添加6％的水湿混3-5分钟，保证混合好的料具有良好的成型性能。
(3)压制成型
将混合好的料倒入模具中(模具尺寸设计按照用户提出的形状要求进行设计)，使模具均匀充满。采用液压机压制成型，出模后自然养护24h。
(4)高温烧制
将样品放入烧结炉中进行烧制，室温升至1300℃，按10℃/分钟进行升温；高温点控制在1300℃，保温时间为8小时；1300℃降至室温，按10℃/分钟进行降温，冷却后得到堇青石多孔陶瓷产品。
(5)指标检测
按GB/T4741-1999陶瓷材料抗弯强度试验方法、GB/T3810.3-1999陶瓷材料显气孔率试验方法对堇青石多孔陶瓷产品进行检测，抗弯强度为6MPa，显气孔率为35％。
表4堇青石多孔陶瓷生产配比
原料名称 配比/％
石英砂粉 49
氧化铝微粉 36
97牌号电熔镁砂粉 15
铝酸盐水泥(外加) 4
木屑(外加) 5
钛白粉(外加) 6
水(外加) 6
实施例2
(1)磨料和配料
先采用球磨机分别将97电熔镁砂、石英砂磨制成粒度≤0.088mm，再将磨细后97电熔镁砂、磨细后石英砂粉、氧化铝微粉、铝酸盐水泥、钛白粉和木屑按表5配方准确称量。
(2)混合
采用强制搅拌机先将称量好的物料干混5-8分钟，再添加6％的水湿混3-5分钟，保证混合好的料具有良好的成型性能。
(3)压制成型
将混合好的料倒入模具中(模具尺寸设计按照用户提出的形状要求进行设计)，使模具均匀充满。采用液压机压制成型，出模后自然养护24h。
(4)高温烧制
将样品放入烧结炉中进行烧制，室温升至1300℃，按10℃/分钟进行升温；高温点控制在1300℃，保温时间为8小时；1300℃降至室温，按10℃/分钟进行降温，冷却后得到堇青石多孔陶瓷产品。
(5)指标检测
按GB/T4741-1999陶瓷材料抗弯强度试验方法、GB/T3810.3-1999陶瓷材料显气孔率试验方法对堇青石多孔陶瓷产品进行检测，抗弯强度为7MPa，显气孔率为34％。
表5堇青石多孔陶瓷生产配比
原料名称 配比/％
石英砂粉 49
氧化铝微粉 36
97牌号电熔镁砂粉 15
铝酸盐水泥(外加) 4
木屑(外加) 5
钛白粉(外加) 8
水(外加) 6

Claims (10)

1.堇青石多孔陶瓷的制备方法，其特征在于：包括以下步骤：将石英砂粉、氧化铝微粉、97牌号电熔镁砂粉、结合剂、矿化剂和造孔剂混合均匀，加水，再混合均匀，得半干状态物料；将半干状态物料倒入模具中成型为半成品，半成品经煅烧，得堇青石多孔陶瓷；所述结合剂为铝酸盐水泥，所述矿化剂为钛白粉。
2.根据权利要求1所述的堇青石多孔陶瓷的制备方法，其特征在于：所述造孔剂为碳化硅、淀粉、石墨粉、木屑或植物纤维中的至少一种；进一步的，所述造孔剂的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的4～7％。
3.根据权利要求1或2所述的堇青石多孔陶瓷的制备方法，其特征在于：所述石英砂粉中SiO2≥98％；所述氧化铝微粉中Al2O3≥99％；所述97牌号电熔镁砂中MgO≥97％。
4.根据权利要求1～3任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：所述石英砂粉的粒度≤0.088mm；所述97牌号电熔镁砂粉的粒度≤0.088mm；所述碳化硅的粒度≤0.088mm。
5.根据权利要求1～4任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：各原料含水量在2％以下。
6.根据权利要求1～5任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：所述铝酸盐水泥的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的4～6％。
7.根据权利要求1～6任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：所述钛白粉的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的4～7％。
8.根据权利要求1～7任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：所述水的添加量为石英砂粉、氧化铝微粉、97牌号电熔镁砂粉三者总质量的6～9％。
9.根据权利要求1～8任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：所述成型的压力为15～25MPa，保压5～10s。
10.根据权利要求1～9任一项所述的堇青石多孔陶瓷的制备方法，其特征在于：所述煅烧的温度为1250～1350℃，时间为5～10h；优选的，所述煅烧的温度和时间为1300℃×8h。
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