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聚丙烯纤维、偏高岭土和细砂对水硬石灰改性的研究

  • 杨隽永

    机 构：

    南京博物院,江苏南京 210016

    ×
  • ， 冯向伟

    机 构：

    南京博物院,江苏南京 210016

    ×

南京博物院,江苏南京 210016；

Research on the modification of hydraulic lime by polypropylene fiber,metakaolin and fine sand

Nanjing Museum, Nanjing 210016 , China；

作者简介:

杨隽永(1980—),2006年毕业于南京大学地质工程专业,研究方向为无机文物保护,副研究馆员,E-mail:32648167@qq.com

中图分类号:K879.1

文献标识码:A

文章编号:1005-1538(2022)04-0072-08

DOI:10.16334/j.cnki.cn31-1652/k.20211002280

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目录contents

    摘要

    为改善水硬石灰的力学性能,适当提高其抗压与抗折强度,本工作设计并制备了添加不同配比的聚丙烯纤维、偏高岭土和细砂的水硬石灰,并对其力学强度,矿物成分和微观形貌进行试验研究。结果表明,单独添加30%偏高岭土、0.1%聚丙烯纤维或者50%石英砂的水硬石灰抗压强度相对较高。在偏高岭土-水硬石灰中,单独添加0.1%短长度聚丙烯纤维或者共同加入0.1%聚丙烯纤维和50%石英砂可以提高其长期抗压强度。添加聚丙烯纤维还可以提高水硬石灰抗折强度。钙铝水合物不稳定和长期抗压强度下降有关,添加1%聚丙烯纤维可以提高碳酸化反应。聚丙烯纤维还能够增大水硬石灰内部的摩擦力和锚固力。在南京市罗廊巷太平天国建筑壁画保护中,对于地仗层脱落部位的修补采用改性水硬石灰进行了局部应用,效果良好。

    Abstract

    In order to improve the mechanical properties of hydraulic lime and to appropriately increase its compressive and flexural strength, we designed and prepared hydraulic lime with different proportions of polypropylene fiber, metakaolin and fine sand, and experimentally studied the mechanical strength, mineral composition and morphology of each mixture. The results show that the compressive strengths of hydraulic lime mixtures containing 30% metakaolin, 0.1% polypropylene fiber or 50% quartz sand only are relatively higher. Metakaolin-hydraulic lime presents improved long-term compressive strength when 0.1% short-length polypropylene fiber is added alone or 0.1% polypropylene fiber and 50% quartz sand are added together. The flexural strength of hydraulic lime containing polypropylene fiber is also increased. The decrease of long-term compressive strength is related to the instability of calcium-aluminum hydrate, and the carbonation reaction can be increased by adding 1% polypropylene fiber. The friction and anchoring forces can also be increased by adding polypropylene fiber. Modified hydraulic lime was used in the conservation of architectural murals of the Taiping Heavenly Kingdom at Luolang Lane in Nanjing. Its application to the local restoration of ground layers achieved good effects.

  • 0 引言

  • 水硬石灰作为传统的硅酸盐建筑材料在我国使用已有千年历史[1]。从早期的烧料礓石、烧阿嘎土[2]到后来《天工开物》中记载“风吹成粉”工法得到的石灰[3]都具有水硬性成分。水硬石灰中除了气硬性组分氧化钙外,还有水硬性组分β-硅酸钙(β-CaSiO3)及铝硅酸钙(Ca2Al2(SiO3)5)[2],因此能在潮湿环境中胶结凝固。

  • 水硬石灰常添加其他材料在不同场景中使用。添加偏高岭土可以提高其早期强度、长期力学性能和耐水性能[4-13]。偏高岭土是由高岭石[Al2Si2O5(OH)4]通过高温煅烧(600~850℃)脱水形成的具有较高火山灰活性的无水硅酸铝(Al2O3·2SiO2),极易与石灰等碱性物质发生反应,影响石灰的水化和碳酸化进程[10-11]。添加纤维材料可以提高界面摩擦作用力,在石灰周围形成“锚固区”[14-20],从而提高抗拉强度。添加细砂起到填充和骨架作用,增加胶凝材料密度,改变孔隙结构,是“三合土”和砂浆砌体常用配方[21-23]。

  • 关于水硬石灰胶凝材料的改性研究较多,但是对于不同原料共同配比的研究相对较少。本研究首先在水硬石灰中单独添加偏高岭土、细砂以及聚丙烯纤维,然后在此基础上研究添加聚丙烯纤维和石英砂的偏高岭土-水硬石灰,通过恒温恒湿环境中养护后测量其力学性能、矿物特性和微观形貌,得出多组适宜的水硬石灰胶凝配比。最后在南京市罗廊巷太平天国建筑壁画地仗层脱落部位的局部修补中使用改性水硬石灰,取得较好的效果。

  • 1 材料和方法

  • 1.1 实验材料

  • 试验所用水硬石灰是从上海德赛堡建筑材料有限公司购买的进口天然水硬石灰(型号为NHL2),化学组成见表1。偏高岭土(MK)购置于信墨实业,主要成分Al2O3(45%±2%)和SiO2(52%±2%),平均粒度1250目。聚丙烯纤维(PPF)购于汇祥纤维工厂,选择6,12mm两种长度的纤维,主要技术参数见表2。石英砂(quartz sand)购于优索样品,平均粒度100目,标准砂(standard sand)为厦门艾斯欧产品,试验用水为纯净水。

  • 表1 NHL2的化学组成

  • Table1 Chemical composition of NHL2

  • 表2 聚丙烯纤维的主要技术参数

  • Table2 Main technical parameters of polypropylene fiber

  • 1.2 材料配比

  • 首先,将水硬石灰分别与偏高岭土、石英砂(或标准砂)或聚丙烯纤维按照不同比例混合制样。其中偏高岭土与水硬石灰的质量比为0∶10、1∶9和3∶7,水硬石灰与石英砂或标准砂的质量比为1∶1、1∶2,不同长度(6mm、12mm)聚丙烯纤维添加量分别为0.1%、0.3%、0.5%、1.0%。然后,在水硬石灰-偏高岭土中添加聚丙烯纤维和石英砂,材料配比和样品编号见表3。试验中水灰比统一为0.65,含砂样品中水灰比不包括砂粒。

  • 表3 样品编号和材料配比

  • Table3 Sample number and material ratio

  • 注:aggregate=SS or QS; SS=Standard sand, QS=Quartz sand; PS=Φ(6mm)PPF, PL=Φ(12mm)PPF。

  • 1.3 样品制备

  • 按照《建筑砂浆基本性能试验方法标准》制作抗压强度样品,尺寸为70.7mm×70.7mm×70.7mm,按照《水泥胶砂强度检验方法(ISO法)》制作抗折强度样品,尺寸为40mm×40mm×160mm。试样制备完成后24h脱模,然后将样品放入恒温恒湿柜内,在25℃和相对湿度95%±5%的环境中进行养护。为提高效率同时保证结果有代表性,制作所有配比的抗压强度试块,抗折强度则选择部分配比进行制作。每个龄期样品数量为3块,结果取平均值。

  • 1.4 实验方法

  • 按照《建筑砂浆基本性能试验方法标准》和《水泥胶砂强度检验方法(ISO法)》标准进行抗压和抗拉强度测试,测试机器为CMT5105型微机控制电子万能试验机(WX146)。XRD测试仪器为帕纳科,工作电压为40kV,工作电流40mA,靶材为Cu靶,SEM测试仪器为日立S3400,测试电压为20.0kV。

  • 2 结果与讨论

  • 2.1 添加偏高岭土对水硬石灰力学强度的影响

  • 图1为不同偏高岭土掺量的水硬石灰样品在28d,90d,180d的抗压与抗折强度变化。在此次实验养护条件中,NHL2在28d,90d,180d龄期的抗压强度分别为1.6,2.91,2.76MPa,同样龄期的NMK1和NMK2的抗压强度则分别达到了2.40,4.11,4.06MPa以及4.84,6.98,6.90MPa。由此可知添加偏高岭土可以提高水硬石灰的抗压强度,并且在90d龄期时抗压强度可能已达到峰值。

  • 图1 添加偏高岭土的水硬石灰抗压与抗折强度

  • Fig.1 Compressive and flexural strength of hydraulic lime with metakaolin

  • 抗折强度也随着龄期增加而逐渐提高。其中NHL2在28d,90d,180d龄期的抗折强度分别为0.277,0.717,1.53MPa,添加偏高岭土的样品NMK1和NMK2抗折强度则分别达到了0.302,1.41,1.83MPa和0.708,1.53,2.26MPa。

  • 在试验操作中可以发现,往水硬石灰中添加偏高岭土越多拌和会越困难,因此在此次水灰比时偏高岭土添加量不宜超过30%。

  • 2.2 添加细砂对水硬石灰力学强度的影响

  • 添加细砂对水硬石灰强度的影响如图2所示。从此次试验结果来看,其抗压强度在不同砂粒类型以及砂粒含量时表现出不同特点:当砂粒与水硬石灰质量相同时,含有石英砂的水硬石灰样品抗压强度更高;当砂粒质量为水硬石灰的2倍时,含有标准砂的水硬石灰样品抗压强度略高。所有样品中,石英砂和水硬石灰质量相等时抗压强度最高。对于抗折强度而言,当砂粒与水硬石灰质量相同时,添加石英砂的水硬石灰样品抗折强度略低。在90~180d期间抗压、抗折强度均在增加。

  • 含有细砂的水硬石灰样品强度来源包括细砂和水硬石灰水化产物两部分,前者与砂粒填充密实度有关,后者则与反应时间、反应量、反应程度有关。NHL2的粒径在1~10 μm之间[24],标准砂的粒径区间为150 μm~4.75mm,100目石英砂的粒径为150 μm。在相同质量下,砂粒越多或者粗砂粒越少,细砂填充密实度越大。此外如果细砂越多,水硬石灰则越少,水化反应产物也越少,两种因素此消彼长。这些可能是其抗压强度变动的原因之一。

  • 图2 添加细砂的水硬石灰抗压与抗折强度

  • Fig.2 Compressive and flexural strength of hydraulic lime with fine sand

  • 2.3 添加聚丙烯纤维对水硬石灰力学强度的影响

  • 图3和图4为添加不同长度与含量聚丙烯纤维的水硬石灰灰浆样品在不同龄期的抗压与抗折强度变化。由此可知,添加聚丙烯纤维可以明显提高水硬石灰的抗压与抗折强度,而且从90d到180d抗压强度仍在增加,说明纤维在抗压强度中一直起到一定作用。在180d后添加0.1%的短纤维抗压强度最高(为5.38MPa),其次是添加0.1%和0.3%长纤维后的抗压强度(分别为4.98MPa,4.96MPa)。抗折强度在180d后,添加0.1%的短纤维和长纤维的样品分别达到1.86MPa和2.08MPa。

  • 图3 添加短纤维的水硬石灰抗压和抗折强度

  • Fig.3 Compressive and flexural strength of hydraulic lime with short polypropylene fiber

  • 在本次试验配比的研究范围中,随着聚丙烯纤维的掺量增加,水硬石灰的抗压强度先增大后减小然后再增大。当聚丙烯纤维掺量较少时,石灰会在纤维表面包裹,并通过界面摩擦作用增加粘结力,同时纤维在石灰周围形成“锚固区”,增加了纤维的传递荷载和抗拉能力[19-22]。添加更多纤维时,纤维容易团聚,会在石灰基体中产生空隙,破坏其整体性[23],因此降低抗压强度。但是继续增加纤维后,原本空隙部位被纤维填充,通过纤维连接将石灰基体固定,故还可以增加抗压强度。

  • 图4 添加长纤维的水硬石灰抗压和抗折强度

  • Fig.4 Compressive and flexural strength of hydraulic lime with long polypropylene fiber

  • 2.4 添加聚丙烯纤维和石英砂对偏高岭土-水硬石灰力学强度的影响

  • 图5为在偏高岭土-水硬石灰中添加0.1%含量,不同长度(6mm和12mm)聚丙烯纤维的抗压强度与抗折强度变化。由此可知,添加纤维后的样品抗压强度在28~180d都在增加,其中添加短纤维的样品抗压强度比未添加时有所提高,而添加长纤维时则略有降低。抗折强度在添加纤维后都明显提高,相对而言添加短纤维后抗折强度略高。

  • 图5 含纤维的偏高岭土-水硬石灰抗压和抗折强度

  • Fig.5 Compressive and flexural strength of metakaolin-hydraulic lime with polypropylene fiber

  • 图6为在偏高岭土-水硬石灰中添加0.1%含量,不同长度(6mm和12mm)聚丙烯纤维以及50%石英砂的抗压与抗折强度变化。由此可知,虽然短期状态中其抗压强度比未添加时略低,但长期状态中则持平或略高。关键点在于,此时抗折强度比未添加时均明显提高。

  • 图6 含纤维和石英砂的偏高岭土-水硬石灰抗压和抗折强度

  • Fig.6 Compressive and flexural strength of metakaolin-hydraulic lime with polypropylene fiber and quartz sand

  • 2.5 矿物成分分析

  • 图7为添加不同偏高岭土的水硬石灰样品中矿物成分的变化。反应产物中主要矿物为碳酸钙和氢氧化钙,此外还有部分石英、水化铝酸四钙、单碳水化铝酸钙、钙矾石、斜硅钙石等。其中钙铝水合物与水硬石灰和偏高岭土的火山灰反应有关,另外球雯石型碳酸钙也是添加偏高岭土后特有的产物之一[6]。

  • 图7 水硬石灰与含偏高岭土的水硬石灰XRD图谱

  • Fig.7 XRD patterns of hydraulic lime with or without metakaolin

  • 随着龄期的增长,碳酸化反应不断进行,反应产物中碳酸钙与氢氧化钙的比例逐渐变大。随着偏高岭土增多,火山灰反应变强,也使得氢氧化钙含量不断减少。钙铝水合物的不稳定性是影响抗压强度在180d时有所下降的一个重要原因[6]。

  • 图8为添加不同含量聚丙烯纤维的水硬石灰样品中矿物成分的变化。添加少量纤维时样品的水化反应的矿物成分没有明显改变,但是添加较多纤维时样品在180d后水化反应产物中氢氧化钙明显减少。这可能与纤维增多后导致孔隙增大使得样品内部碳酸化反应变多有关。

  • 2.6 微观结构分析

  • 图9为90d龄期添加不同比例偏高岭土的水硬石灰灰浆样品SEM结果。结合XRD数据和相关文献[6,25-26]可知,此时纯水硬石灰内部有较多针状的2CaO·SiO2的水合物晶体和片状的氢氧化钙,碳酸钙晶体还较少,孔隙较多。NMK1样品内针状和片状晶体减少,蜂窝状CaCO3晶体增多。NMK2样品针状2CaO·SiO2的水合物晶体变为骨头状,CaCO3重结晶体进一步增大,形成致密的网络状结构,孔隙减小,因此力学强度更高。图10为添加质量0.1%、长度6mm和12mm聚丙烯纤维的水硬石灰灰浆样品在90d龄期SEM结果。此时聚丙烯纤维和水硬石灰水化产物之间产生铆合作用,增大破坏所需作用力,同时可以起到拉伸作用,防止外力载荷对水硬石灰灰浆总体结构的较大破坏。

  • 图8 添加聚丙烯纤维的水硬石灰XRD图谱

  • Fig.8 XRD patterns of hydraulic lime with polypropylene fiber

  • 图9 水硬石灰与含偏高岭土的水硬石灰90d时SEM图像

  • Fig.9 SEM images of hydraulic lime with or without metakaolin after 90days

  • 图10 添加质量0.1%、长度6mm(左侧)和12mm(右侧)聚丙烯纤维的水硬石灰在90d时SEM图像

  • Fig.10 SEM images of hydraulic lime with 0.1%polypropylene fiber by mass of 6mm (left) and 12mm (right)in length after 90days

  • 3 案例应用

  • 南京市罗廊巷太平天国建筑壁画位于太平天国东王府遗址范围内,原有十幅砖体壁画,现仅存两幅。由于保存不善,壁画出现龟裂起甲,地仗层空鼓酥碱、空鼓和缺失等病害。2020年4月南京博物院依据壁画保护方案展开施工,其中需要对地仗层缺失部分进行修补。经设计单位检测原壁画地仗层主要为加了植物秸秆的石灰,且含有少量石英砂和石膏,厚度约7mm。在现场施工时采用了添加30%高岭土和0.1%聚丙烯纤维的水硬石灰进行局部修复,观察一年后表面未开裂(图11),证明保护效果较好。

  • 图11 南京罗廊巷太平天国建筑壁画地仗层修补

  • Fig.11 Restoration of ground layers of architectural murals of the Taiping Heavenly Kingdom at Luolang Lane in Nanjing

  • 4 结论

  • 1)在水硬石灰中单独添加偏高岭土、聚丙烯纤维和细砂或者在偏高岭土-水硬石灰中添加聚丙烯纤维或者细砂可以适当提高其抗压强度。但是对于天然水硬石灰不宜一味追求高强度设计,否则在完全固化后其强度远高于基体强度会产生次生破坏。

  • 2)添加偏高岭土可以通过火山灰反应和碳酸化反应增加碳酸钙含量,从而适当提高水硬石灰的抗压强度。在此试验的水灰比中,添加30%的偏高岭土的强度最高。钙铝水合物不稳定性会导致其长期抗压强度略有下降。添加不同细砂的水硬石灰抗压强度与细砂填充密实度和水硬石灰水化产物有关,试验中当石英砂与水硬石灰质量比为1时抗压强度相对较高。添加0.1%聚丙烯纤维的水硬石灰抗压强度相对较高,且抗压强度随龄期不断增长,受压破坏时变形较小;

  • 3)在偏高岭土-水硬石灰中添加0.1%短长度聚丙烯纤维或者共同加入0.1%聚丙烯纤维和50%石英砂可以提高其长期抗压强度。

  • 4)添加聚丙烯纤维可以增大水硬石灰内部摩擦力和锚固力,提高其抗折强度,从而增加石灰材料的韧性。

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  • 基本信息

    中图分类号: K879.1
    文献标识码: A
    DOI: 10.16334/j.cnki.cn31-1652/k.20211002280
    文章编号: 1005-1538(2022)04-0072-08

    基金信息

    江苏省科技厅社会发展面上项目资助(BE2020730)；

    引用信息

    稿件历史

    收稿日期: 2021-10-17

  • 参考文献

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