CN109081689A - 一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法 - Google Patents

一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法 Download PDF

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CN109081689A
CN109081689A CN201810981832.4A CN201810981832A CN109081689A CN 109081689 A CN109081689 A CN 109081689A CN 201810981832 A CN201810981832 A CN 201810981832A CN 109081689 A CN109081689 A CN 109081689A
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opoka
cordierite ceramic
alumina fibre
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郭元
章波
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Wuhu Corey Yuen New Mstar Technology Ltd
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Abstract

本发明涉及一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，包括以下步骤：（1）按按照改性蛋白土：氧化铝粉：氧化铝纤维：氧化镁：烧结助剂的重量比55:25:5:14:1的比例，原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；（2）然后加入粉料10wt%的粘结剂，然后加入去离子水，调配固含量为50%的陶瓷浆料；（3）后将制成的膏体塞入模具中，采用压力机模干压成型，其成型压力为20ΜPa，保压2 min将粉料压制成型，然后自然干燥24h，得陶瓷坯料；（4）将陶瓷坯料烧结，即得堇青石陶瓷。本发明的烧结助剂采用生滑石、长石、高岭土、氧化铈、白和钛白粉，并且其进行除杂和烧结处理，使得得到的烧结助剂具有优良的性能，能够有效的降低堇青石陶瓷的烧结温度，提高机械强度，降低热膨胀系数。

Description

一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法
技术领域
本发明涉及一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，属于无机陶瓷材料领域。
背景技术
堇青石陶瓷具有较高强度、优异的化学稳定性和低的热膨胀,可作为汽车尾气处理器载体的首选材料。人工合成堇青石粉体是堇青石制品原料的主要来源。利用天然矿物材料，如滑石、高岭土、蒙脱石等为原料合成堇青石陶瓷工艺及其性能的研究受到广泛关注。高纯度氧化物合成堇青石是利用高纯度的MgO、SiO2和Al2O3通过高温固相合成反应进行制备堇青石，也是最传统的制备方法。这种方法具有产物纯度高，合成转化率高等特点。天然矿物合成堇青石具有原料来源广，成本低，便于工业化生产等特点。通过在这种方法可以使用的原料有滑石、硅藻土、长石和高岭土等。申请公布号CN102584191A，发明名称：用蛇纹石尾矿制制备堇青石陶瓷的方法，采蛇纹石尾矿和高岭土尾矿为主要原料，同时加入少量的工艺氧化铝，通过球磨、压制成型、干燥和烧结工艺，制备出堇青石陶瓷材料。该发明不仅解决了尾矿大量堆积对环境的污染问题，而且能使产品降低原料成本，制备过程简单，易于控制，并且烧结温度低，适合于工业化生产。但是该方法制备的堇青石的气孔率低、强度低、热膨胀系数高。
发明内容
本发明提供了一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，解决了现有堇青石陶瓷气孔率低、强度低和热膨胀系数高等问题。
为解决上述技术问题，本发明采用的技术方案为：
一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土：氧化铝粉：氧化铝纤维：氧化镁：烧结助剂的重量比55:25:5:14:1的比例，原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)然后加入粉料10wt％的粘结剂，然后加入去离子水，调配固含量为50％的陶瓷浆料；
(3)后将制成的膏体塞入模具中，采用压力机模干压成型，其成型压力为20ΜPa，保压2min将粉料压制成型，然后自然干燥24h，得陶瓷坯料；
(4)将陶瓷坯料烧结，即得堇青石陶瓷。
进一步，本发明的一种优选方案为：所述的烧结助剂，按照重量份计，包括30-40份滑石、20-30份长石、20-30份高岭土、1份氧化铈、3-5份钛白粉。
进一步，本发明的一种优选方案为：所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
进一步，本发明的一种优选方案为：所述的烧结为以1℃/min的速率缓慢升温至300℃，保温2小时，然后以2℃/min，升温至800℃，保温2小时，5℃/min升至1350℃保温4小时烧结，然后随炉冷却。
进一步，本发明的一种优选方案为：所述的烧结助剂的制备方法：(1)将滑石、长石、高岭土分别600℃焙烧2h后，按照液固比为4∶1加入浓度为30％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的滑石、长石、高岭土、氧化铈和钛白粉混合均匀，然后4℃/min升至1300℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
本发明的有益效果：
本发明通过添加烧结助剂，烧结助剂采用生滑石、长石、高岭土、氧化铈、白和钛白粉，并且其进行除杂和烧结处理，使得得到的烧结助剂具有优良的性能，能够有效的降低堇青石陶瓷的烧结温度，提高机械强度，降低热膨胀系数。
蛋白土又称蛋白石，是一种含水非晶质或胶质的活性二氧化硅，是一种无定形硅质矿物。其化学组成为SiO2.nH2O，其中所Si为无定形结构，主要成份除Si外还含少量氧化铁、氧化铝、锰、铜和有机杂质等。蛋白石岩是由极微小的蛋白石球体组成，有较发育的孔隙，具有孔隙度高，吸水性强，吸附性好等特点。经过改性处理，SiO2含量由79％升至90％，且空隙率大幅提高。采用蛋白土作为主料，作为造孔剂，可以有效的提高堇青石陶瓷的空隙率，降低粘结剂的用量，进而提高产品的强度。
氧化铝纤维是一种高性能无机纤维，具有长纤、短纤、晶须等多种形式。氧化铝纤维直径10-20μm，密度2.7-4.2g/cm3，强度1.4-2.45GPa，模量190-385GPa，最高使用温度为1100-1400℃。高强度、高模量、极好的耐热性和耐高温氧化性是氧化铝纤维的突出优点。另外氧化铝纤维还拥有热膨胀系数低，抗热震性好，热导率小等优点。与其他纤维相比，氧化铝纤维可以在更高的高温下保持抗拉强度。氧化铝纤维表面活性好，容易与陶瓷基体相匹配。
采用氧化铝纤维与蛋白土复合，一方面可以有效的提高堇青石陶瓷的折弯强度，另一方面可以提高气孔率。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土：氧化铝粉：氧化铝纤维：氧化镁：烧结助剂的重量比55:25:5:14:1的比例，原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)然后加入粉料10wt％的粘结剂，然后加入去离子水，调配固含量为50％的陶瓷浆料；
(3)后将制成的膏体塞入模具中，采用压力机模干压成型，其成型压力为20ΜPa，保压2min将粉料压制成型，然后自然干燥24h，得陶瓷坯料；
(4)将陶瓷坯料烧结，所述的烧结为以1℃/min的速率缓慢升温至300℃，保温2小时，然后以2℃/min，升温至800℃，保温2小时，5℃/min升至1350℃保温4小时烧结，然后随炉冷却，即得堇青石陶瓷。
所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
所述的烧结助剂，按照重量份计，包括30份滑石、30份长石、25份高岭土、1份氧化铈、3份钛白粉。
所述的烧结助剂的制备方法：(1)将滑石、长石、高岭土分别600℃焙烧2h后，按照液固比为4∶1加入浓度为30％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的滑石、长石、高岭土、氧化铈和钛白粉混合均匀，然后4℃/min升至1300℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
实施例2
一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土：氧化铝粉：氧化铝纤维：氧化镁：烧结助剂的重量比55:25:5:14:1的比例，原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)然后加入粉料10wt％的粘结剂，然后加入去离子水，调配固含量为50％的陶瓷浆料；
(3)后将制成的膏体塞入模具中，采用压力机模干压成型，其成型压力为20ΜPa，保压2min将粉料压制成型，然后自然干燥24h，得陶瓷坯料；
(4)将陶瓷坯料烧结，所述的烧结为以1℃/min的速率缓慢升温至300℃，保温2小时，然后以2℃/min，升温至800℃，保温2小时，5℃/min升至1350℃保温4小时烧结，然后随炉冷却，即得堇青石陶瓷。
所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
所述的烧结助剂，按照重量份计，包括35份滑石、25份长石、20份高岭土、1份氧化铈、4份钛白粉。
所述的烧结助剂的制备方法：(1)将滑石、长石、高岭土分别600℃焙烧2h后，按照液固比为4∶1加入浓度为30％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的滑石、长石、高岭土、氧化铈和钛白粉混合均匀，然后4℃/min升至1300℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
实施例3
一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，包括以下步骤：
(1)按照改性蛋白土：氧化铝粉：氧化铝纤维：氧化镁：烧结助剂的重量比55:25:5:14:1的比例，原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
(2)然后加入粉料10wt％的粘结剂，然后加入去离子水，调配固含量为50％的陶瓷浆料；
(3)后将制成的膏体塞入模具中，采用压力机模干压成型，其成型压力为20ΜPa，保压2min将粉料压制成型，然后自然干燥24h，得陶瓷坯料；
(4)将陶瓷坯料烧结，所述的烧结为以1℃/min的速率缓慢升温至300℃，保温2小时，然后以2℃/min，升温至800℃，保温2小时，5℃/min升至1350℃保温4小时烧结，然后随炉冷却，即得堇青石陶瓷。
所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为3∶1加入浓度为40％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
所述的烧结助剂，按照重量份计，包括40份滑石、20份长石、30份高岭土、1份氧化铈、5份钛白粉。
所述的烧结助剂的制备方法：(1)将滑石、长石、高岭土分别600℃焙烧2h后，按照液固比为4∶1加入浓度为30％硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；(2)将处理后的滑石、长石、高岭土、氧化铈和钛白粉混合均匀，然后4℃/min升至1300℃保温3小时烧结，然后随炉冷却；(4)将得到的烧结物粉碎，球磨，即得烧结助剂。
测定实施例1-3的堇青石陶瓷性能，具体见下表。
热膨胀系数/℃ 开气孔率/％ 抗弯强度/(MPa)
实施例1 1.56×10<sup>-6</sup> 43.2 45.6
实施例2 1.53×10<sup>-6</sup> 42.3 44.8
实施例3 1.51×10<sup>-6</sup> 43.2 44.9
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (5)

1.一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，其特征在于，包括以下步骤：
（1）按照改性蛋白土：氧化铝粉：氧化铝纤维：氧化镁：烧结助剂的重量比55:25:5:14:1的比例，原料放入玛瑙球磨罐中，用行星球磨机以300rpm球磨3h，得到混合均匀的粉料；
（2）然后加入粉料10wt%的粘结剂，然后加入去离子水，调配固含量为50%的陶瓷浆料；
（3）后将制成的膏体塞入模具中，采用压力机模干压成型，其成型压力为20ΜPa，保压2min将粉料压制成型，然后自然干燥24h，得陶瓷坯料；
（4）将陶瓷坯料烧结，即得堇青石陶瓷。
2.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备堇青石陶瓷的方法，其特征在于：所述的烧结助剂，按照重量份计，包括30-40份滑石、20-30份长石、20-30份高岭土、1份氧化铈、3-5份钛白粉。
3.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备堇青石陶瓷，其特征在于：
所述的改性蛋白土的制备方法为称取一定量蛋白土600℃焙烧2h后，按照液固比为 3∶1加入浓度为 40%硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥。
4.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备堇青石陶瓷，其特征在于：所述的烧结为以1℃/min 的速率缓慢升温至 300℃，保温2小时，然后以2℃/min，升温至800℃，保温2小时， 5℃ /min升至 1350℃保温4小时烧结，然后随炉冷却。
5.根据权利要求1所述的一种氧化铝纤维增强蛋白土制备堇青石陶瓷，其特征在于：所述的烧结助剂的制备方法：（1）将滑石、长石、高岭土分别600℃焙烧2h后，按照液固比为 4∶1加入浓度为30%硫酸，搅拌均匀，100℃，反应2h，然后用水冲洗至无硫酸，干燥；（2）将处理后的滑石、长石、高岭土、氧化铈和钛白粉混合均匀，然后4℃ /min升至 1300℃保温3小时烧结，然后随炉冷却；（4）将得到的烧结物粉碎，球磨，即得烧结助剂。
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