基于动态模量成像的硬化水泥浆体微观物相的识别*

doi:10.11901/1005.3093.2015.468

材料研究学报

2016, Vol. 30

Issue (5): 321-328 DOI: 10.11901/1005.3093.2015.468

本期目录 | 过刊浏览

基于动态模量成像的硬化水泥浆体微观物相的识别*

高翔^1,², 魏亚¹(

), 黄卫²

1. 清华大学土木工程系土木工程安全与耐久教育部重点实验室北京 100084
2. 东南大学教育部智能运输系统研究中心南京 210096

Phase Identification in Cement Paste by Modulus Mapping

GAO Xiang^1,², WEI Ya^1,^**(

), HUANG Wei²

1. Key Laboratory of Civil Engineering Safety of Durability of China Education Ministry, Department of Civil Engineering, Tsinghua University, Beijing 100084, China
2. Ministry of Education ITS Engineering Research Center, Southeast University, Nanjing 210096, China

引用本文:

高翔, 魏亚, 黄卫. 基于动态模量成像的硬化水泥浆体微观物相的识别*[J]. 材料研究学报, 2016, 30(5): 321-328.
Xiang GAO, Ya WEI, Wei HUANG. Phase Identification in Cement Paste by Modulus Mapping[J]. Chinese Journal of Materials Research, 2016, 30(5): 321-328.

全文: PDF(3833 KB) HTML

摘要:

使用动态力学分析的模量成像技术对硬化水泥净浆进行微观层次上的物相识别, 根据不同物相弹性性质的差异得到了目标区域的储能模量图, 辅以形貌观测、成分分析和原位静态压痕手段, 准确识别了未水化颗粒及其周边的高密度(High density, HD)和低密度(Low density, LD)CSH凝胶。结果表明, HD CSH凝胶和LD CSH凝胶的化学成分一致, 其各自的典型动态模量分别为36GPa和24GPa, 具有较好的区分度, 且该值与同样表征物相弹性性质的压痕模量数值近似, 动态模量成像图可给出清晰的物相边界。用该方法分析硬化水泥浆体微观性能, 可避免由于不能准确定位各物相而引起盲目性和重复工作, 有助于有的放矢地研究目标物相。

关键词 ：无机非金属材料, 硬化水泥浆体, 动态力学分析, 模量成像, 物相识别, CSH凝胶, 储能模量

Abstract：

Phases in cement paste can be identified in micro scale by dynamic mechanical analysis (DMA) based modulus mapping owing to the characteristics of this technique: rapid, precise, high resolution and non-destructive. According to the storage modulus mapping which reflects the differences of elastic properties, the unhydrated clinker, as well as the high density calcium silicate hydrate (CSH) gel and low density CSH gel, which surrounded the clinker can be recognized with the assistance of morphology observation, components analysis and in-situ static indentation etc. Results show that the chemical composition of HD CSH and LD CSH is the same, while their storage modulus are 36GPa and 24GPa respectively, and the phase identification can be accomplished by taking the individual storage modulus into account. Therefore, blindness and repetition in traditional experiments can be avoided by employing the method of DMA-based modulus mapping, and then the properties of interested phase can be acquired with targeted approach.

Key words： inorganic non-metallic materials cement paste dynamic mechanical analysis modulus mapping phase identification CSH gel storage modulus

收稿日期: 2015-08-20

ZTFLH:

TB321

基金资助:* 国家自然科学基金51578316资助项目

作者简介: 本文联系人: 魏亚

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图1 动态纳米压入原理示意图

图2 典型荷载-压入深度曲线

表1 原材料化学组成(质量分数, %)

图3 AFM拍摄试件表面粗糙度

图4 动态模量图像及光镜图、形貌图和三维图

图5 纵线上储能模量随位置的变化

表2 纵线上两相水化产物储能模量值对比

图6 研究区域(约30 μm×30 μm)形貌图及EDS/NI试验示意图

图7 静态压入点的力学特征及其与储能模量的对照

图8 各物相中主要元素占比

图9 EDS测试的Ca/Si比

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