CN108147801A - 一种石墨烯瓷砖烧制方法 - Google Patents
一种石墨烯瓷砖烧制方法 Download PDFInfo
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- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims abstract description 7
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Abstract
本发明公开了一种石墨烯瓷砖烧制方法，本发明以钾长石35份、硅灰石、锂辉石、刚玉粉、凹凸棒土、硅藻土、黄磷矿渣等复配作为石墨烯瓷砖的原料，通过对二氧化硅溶胶中水分的控制依次获得湿坯、干坯，最后烧结，在烧结时，通过胶粒表面硅烷醇基团间发生缩合，从而带动石墨烯瓷砖各成分相互靠拢并聚集，而各成分之间的间隙则由胶粒填充，胶粒间以化学键(Si‑O‑Si)相结合，形成稳定的空间网络结构，将各成分牢固地结合在一起，大大降低气孔形成的可能性，隙率低显著降低，从而可得到低吸水率的石墨烯瓷砖。
Description
技术领域
本发明属于建筑陶瓷材料技术领域，具体涉及一种石墨烯瓷砖烧制方法。
背景技术
陶瓷砖是由粘土、石英砂以及其他无机非金属原料经配料、球磨、制粉、成型、烧结等工艺生产的板状或块状陶瓷制品，广泛应用于装饰与保护建筑物、构筑物的墙面和地面。瓷砖是陶瓷砖中的一种，其吸水率低于0.5％。陶瓷坯体经过高温煅烧后变成致密的烧结体，烧结体上存在许多小气孔，正是这些小气孔使瓷砖具有一定的吸水率。吸水率是直接影响瓷砖粘贴和使用性能，也是评价瓷砖质量优劣的重要指标，吸水率的大小对瓷砖的强度、线性膨胀、抗冻性、抗冲击性等性能都有很大的影响，吸水率较低的瓷砖烧结程度好、强度更高，综合性能指标更优。
陶瓷烧结是指高温条件下，坯体表面积减小，孔隙率降低，机械性能提高的致密化过程。但是现有瓷砖在烧结过程中不可避免地会形成许多小气孔，使得制备的瓷砖吸水率高，坯体疏松，综合性能差。
石墨烯是目前已知强度最高的材料之一，同时还具有很好的韧性，且可以弯曲，石墨烯的理论杨氏模量达1.0TPa，固有的拉伸强度为130GPa。目前已有瓷砖通过添加石墨烯成分来提高强度，但是这种瓷砖仍存在吸水率高的问题。
发明内容
本发明的目的在于：针对上述现有瓷砖烧制方法制得的瓷砖存在孔隙率大，导致吸水率高的问题，本发明提供一种石墨烯瓷砖烧制方法。
本发明采用的技术方案如下：
一种石墨烯瓷砖烧制方法，包括以下步骤：
(1)按重量份计：取钾长石30-50份、硅灰石30-40份、锂辉石20-30份混合均匀，粉碎，湿法球磨，烘干后研细，制得粒径为10-100μm的粉料；
(2)取刚玉粉20-25份、黄磷矿渣5-10份混合均匀，粉碎，湿法球磨，过200-400目筛，喷雾造粒；
(3)将步骤(1)制得的粉料和步骤(2)制得的颗粒加入混料机中混合5-10min，然后加入凹凸棒土10-20份、硅藻土10-15份混合10-20min，获得混合料；
(4)将氧化石墨烯5-10份加入至二氧化硅溶胶50-100份中，搅拌均匀，然后加入步骤(3)制得的混合料，搅拌均匀后于100-120℃条件下真空干燥4-6h，制得湿坯；
(5)将湿坯送入干燥窑中干燥至含水量为3-5％的干坯，干燥窑温度为150-200℃；
(6)将干坯送入窑炉中烧结后出料，即得石墨烯瓷砖，其中，烧结温度为800-1000℃，烧结时间为2-4h。
二氧化硅溶胶加热至110℃时，将失去自由水，加热至140-220℃时，将脱附物理吸附水，当温度升高至400-700℃时，胶粒表面的硅醇间缩聚失水，脱出化学吸附水，形成无定形二氧化硅。当在二氧化硅溶胶中加入钾长石、硅灰石、锂辉石、刚玉粉、凹凸棒土、硅藻土、黄磷矿渣并混合均匀后，使二氧化硅溶胶失去自由水，则胶粒将牢固地附着在钾长石、硅灰石等表面，胶粒间形成硅氧结合，从而将钾长石、硅灰石等各成分紧密地粘合在一起，形成湿坯。湿坯在随后的高温烧结过程中，硅烷醇基团间发生缩合，从而带动石墨烯瓷砖各成分相互靠拢并聚集，而各成分之间的间隙则由胶粒填充，胶粒间以化学键(Si-O-Si)相结合，形成稳定的空间网络结构，将各成分牢固地结合在一起，大大降低气孔形成的可能性，隙率低显著降低，从而可得到低吸水率的石墨烯瓷砖。
进一步地，步骤(2)中，颗粒粒径为0.5-1mm。
进一步地，步骤(4)中，氧化石墨烯的制备方法为：将石墨、高锰酸钾加入至98％的浓硫酸中，搅拌均匀后置于50-80℃下反应5-10h，反应过程中滴加去离子水，然后将滤液抽滤后，进行淋洗、分散、超声、干燥得到氧化石墨烯。
进一步地，步骤(5)中，干燥时间为2-4h。
进一步地，步骤(6)中，烧结温度以15-20℃/min的速率升温至800-1000℃。
综上所述，由于采用了上述技术方案，本发明的有益效果是：本发明通过对二氧化硅溶胶中水分的控制依次获得湿坯、干坯，最后烧结，在烧结时，通过胶粒表面硅烷醇基团间发生缩合，从而带动石墨烯瓷砖各成分相互靠拢并聚集，而各成分之间的间隙则由胶粒填充，胶粒间以化学键(Si-O-Si)相结合，形成稳定的空间网络结构，将各成分牢固地结合在一起，大大降低气孔形成的可能性，隙率低显著降低，从而可得到低吸水率的石墨烯瓷砖。
具体实施方式
本说明书中公开的所有特征，除了互相排斥的特征和/或步骤以外，均可以以任何方式组合。
实施例1
一种石墨烯瓷砖烧制方法，包括以下步骤：
(1)按重量份计：取钾长石40份、硅灰石35份、锂辉石25份混合均匀，粉碎，湿法球磨，烘干后研细，制得粒径为10-100μm的粉料；
(2)取刚玉粉22份、黄磷矿渣8份混合均匀，粉碎，湿法球磨，过200-400目筛，喷雾造粒，颗粒粒径为0.5-1mm；
(3)将步骤(1)制得的粉料和步骤(2)制得的颗粒加入混料机中混合8min，然后加入凹凸棒土15份、硅藻土12份混合13min，获得混合料；
(4)将氧化石墨烯8份加入至二氧化硅溶胶80份中，搅拌均匀，然后加入步骤(3)制得的混合料，搅拌均匀后于110℃条件下真空干燥5h，制得湿坯；
(5)将湿坯送入干燥窑中干燥至含水量为3-5％的干坯，干燥窑温度为180℃，干燥时间为3h；
(6)将干坯送入窑炉中烧结后出料，即得石墨烯瓷砖，其中，烧结温度为900℃，烧结时间为3h，烧结温度以18℃/min的速率升温至900℃，石墨烯瓷砖的吸水率为0.31％。
实施例2
一种石墨烯瓷砖烧制方法，包括以下步骤：
(1)按重量份计：取钾长石30份、硅灰石30份、锂辉石20份混合均匀，粉碎，湿法球磨，烘干后研细，制得粒径为10-100μm的粉料；
(2)取刚玉粉20份、黄磷矿渣5份混合均匀，粉碎，湿法球磨，过200-400目筛，喷雾造粒，颗粒粒径为0.5-1mm；
(3)将步骤(1)制得的粉料和步骤(2)制得的颗粒加入混料机中混合6min，然后加入凹凸棒土10份、硅藻土10份混合10min，获得混合料；
(4)将氧化石墨烯5份加入至二氧化硅溶胶58份中，搅拌均匀，然后加入步骤(3)制得的混合料，搅拌均匀后于100℃条件下真空干燥4h，制得湿坯；
(5)将湿坯送入干燥窑中干燥至含水量为3-5％的干坯，干燥窑温度为155℃，干燥时间为2h；
(6)将干坯送入窑炉中烧结后出料，即得石墨烯瓷砖，其中，烧结温度为820℃，烧结时间为2h，烧结温度以15℃/min的速率升温至820℃，石墨烯瓷砖的吸水率为0.45％。
实施例3
一种石墨烯瓷砖烧制方法，包括以下步骤：
(1)按重量份计：取钾长石50份、硅灰石40份、锂辉石30份混合均匀，粉碎，湿法球磨，烘干后研细，制得粒径为10-100μm的粉料；
(2)取刚玉粉25份、黄磷矿渣10份混合均匀，粉碎，湿法球磨，过200-400目筛，喷雾造粒，颗粒粒径为0.5-1mm；
(3)将步骤(1)制得的粉料和步骤(2)制得的颗粒加入混料机中混合10min，然后加入凹凸棒土20份、硅藻土15份混合20min，获得混合料；
(4)将氧化石墨烯10份加入至二氧化硅溶胶100份中，搅拌均匀，然后加入步骤(3)制得的混合料，搅拌均匀后于120℃条件下真空干燥6h，制得湿坯；
(5)将湿坯送入干燥窑中干燥至含水量为3-5％的干坯，干燥窑温度为200℃，干燥时间为4h；
(6)将干坯送入窑炉中烧结后出料，即得石墨烯瓷砖，其中，烧结温度为1000℃，烧结时间为4h，烧结温度以20℃/min的速率升温至1000℃，石墨烯瓷砖的吸水率为0.32％。
如上所述即为本发明的实施例。本发明不局限于上述实施方式，任何人应该得知在本发明的启示下做出的结构变化，凡是与本发明具有相同或相近的技术方案，均落入本发明的保护范围之内。
Claims (5)
1.一种石墨烯瓷砖烧制方法，其特征在于，包括以下步骤：
(1)按重量份计：取钾长石30-50份、硅灰石30-40份、锂辉石20-30份混合均匀，粉碎，湿法球磨，烘干后研细，制得粒径为10-100μm的粉料；
(2)取刚玉粉20-25份、黄磷矿渣5-10份混合均匀，粉碎，湿法球磨，过200-400目筛，喷雾造粒；
(3)将步骤(1)制得的粉料和步骤(2)制得的颗粒加入混料机中混合5-10min，然后加入凹凸棒土10-20份、硅藻土10-15份混合10-20min，获得混合料；
(4)将氧化石墨烯5-10份加入至二氧化硅溶胶50-100份中，搅拌均匀，然后加入步骤(3)制得的混合料，搅拌均匀后于100-120℃条件下真空干燥4-6h，制得湿坯；
(5)将湿坯送入干燥窑中干燥至含水量为3-5％的干坯，干燥窑温度为150-200℃；
(6)将干坯送入窑炉中烧结后出料，即得石墨烯瓷砖，其中，烧结温度为800-1000℃，烧结时间为2-4h。
2.根据权利要求1所述的一种石墨烯瓷砖烧制方法，其特征在于，所述步骤(2)中，颗粒粒径为0.5-1mm。
3.根据权利要求1所述的一种石墨烯瓷砖烧制方法，其特征在于，所述步骤(4)中，氧化石墨烯的制备方法为：将石墨、高锰酸钾加入至98％的浓硫酸中，搅拌均匀后置于50-80℃下反应5-10h，反应过程中滴加去离子水，然后将滤液抽滤后，进行淋洗、分散、超声、干燥得到氧化石墨烯。
4.根据权利要求1所述的一种石墨烯瓷砖烧制方法，其特征在于，所述步骤(5)中，干燥时间为2-4h。
5.根据权利要求1所述的一种石墨烯瓷砖烧制方法，其特征在于，所述步骤(6)中，烧结温度以15-20℃/min的速率升温至800-1000℃。
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