| Citation: | LI Feng, ZHANG Rong-rong, ZHOU Si-qi, YANG Zhan-ning. Preparation and characterization of carbon nanotubes reinforced volcanic ash-based geopolymer[J]. Journal of Traffic and Transportation Engineering, 2023, 23(2): 153-165. doi: 10.19818/j.cnki.1671-1637.2023.02.011
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Volcanic ash is loose and broken particles of rocks, minerals, and volcanic glass formed by condensation during volcanic eruptions. It is exposed on the surface of volcanic relics and can be obtained directly without blasting. After conventional mineral processing operations such as screening and grinding, it can be used. The mining process is simple and environmentally friendly, and it has the advantages of high chemical activity and low cost. China's volcanic ash resources are widely distributed, and many provinces and regions in the northeast and northwest have huge reserves. Therefore, fully utilizing volcanic ash has a positive effect on environmental protection. At present, there is a certain foundation for the preparation and performance research of volcanic ash base polymers, including raw materials, curing conditions, and the influence of alkali activators on the mechanical properties of geopolymers. Zhou et al[14]Two types of volcanic ash with similar chemical compositions were compared, and it was found that the differences in mineral composition, volcanic ash particle size, and amorphous material content led to significant differences in their mechanical properties; Djobo et al[15]Polymer based on volcanic ash was prepared at different curing temperatures, and the results showed that the mechanical properties of the polymer cured at 80 ℃ were better than those at 27 ℃ in strength and wet dry cycle tests; Ibrahim et al[16]We studied the effect of alkaline activators on the mechanics and microstructure of polymers in volcanic ash bases, and found that the higher the concentration of NaOH, the stronger the resulting geopolymer and the denser the microstructure; Wang et al[17]The compressive strength of the polymer in the volcanic ash base was found to increase first and then decrease with the addition of NaOH, with the highest compressive strength reaching 50.36 MPa.
However, cementitious materials including cement and volcanic ash geopolymers are considered quasi brittle materials due to their low tensile strength and poor strain capacity[18-19]Adding fibers can effectively strengthen and toughen geopolymers. Currently, a large amount of research has been conducted on adding steel fibers, polypropylene fibers, polyethylene fibers, basalt fibers, glass fibers, etc. to cementitious materials[20-22]Nanofibers, especially carbon nanotubes, due to their small size, high strength and hardness, and large aspect ratio, can improve the mechanical and fracture properties of materials at the nanoscale[23]Gradually attracting the attention of scholars. At present, research on carbon nanotube reinforced cement materials is very extensive, and the results show that significant performance improvement can be achieved with a mass dosage of only 0.10%. However, there is relatively little research on the nano reinforcement of geopolymer. According to statistics, from 2010 to 2020, only 8% of research on nano material reinforced geopolymers focused on carbon nanotubes[24]Abbasi et al[25]It was found that multi walled carbon nanotubes (MWCNTs) can increase the flexural and compressive strength of polymers based on metakaolin by 28% and 32%, respectively; Saafi et al[26]By adding MWCNTs to fly ash based polymers, the final flexural strength, Young's modulus, and flexural toughness were increased by 1.60, 1.09, and 2.75 times, respectively, with a more significant effect; Li et al[27-28]The conclusion is that MWCNTs enhance the flexural and compressive strength while reducing the water absorption capacity of the material by simultaneously adding MWCNTs and slag to the fly ash based polymer; Khater et al[29]The effect of MWCNTs on the properties of slag based polymer mortar was studied, and it was found that the addition of MWCNTs can improve the structure of the product; Rovnan í k and others[30-31]MWCNTs were added to fly ash based and slag based polymers, and the optimal dosages were found to be 0.15% and 0.10% in the two substrates, respectively. The 28 day compressive strength was increased by 70% and 27%, respectively.
In summary, compared to cement with stable quality control, the precursor of geopolymer is mainly solid waste, with a wide range of sources and unstable physical and chemical properties. Moreover, the use of various types of alkali activators makes the geopolymer reaction environment more complex and variable. These factors have led to the unclear effectiveness and mechanism of MWCNTs in geopolymer. At the same time, research on MWCNTs reinforced geopolymers is very limited and mainly focuses on kaolin based, fly ash based, and slag based polymers. There is little research on volcanic base polymers. Therefore, it is of great significance to carry out the preparation and performance research of carbon nanotube reinforced volcanic ash base polymers. This article first characterized the dispersion of MWCNTs with different ultrasonic durations using a microscope, and then studied the effects of three dosages (0.05%, 0.10%, 0.15%) and three types (original, carboxylated, hydroxylated) of MWCNTs mixed with two materials in order on the viscosity and mechanical properties (flexural strength and compressive strength) of the geopolymer. At the same time, the strengthening mechanism of MWCNTs was revealed by combining the microstructure of MWCNTs in the geopolymer and the results of mercury intrusion tests.
The volcanic slag used in this article was taken from the volcanic group in Huinan County, Jilin Province. Before the experiment began, the volcanic slag was dried and ball milled to obtain volcanic ash powder. The phase composition of volcanic ash was characterized using X-ray Powder Diffraction (XRD), and the results are as follows:Figure 1As shown, the raw materials contain a large amount of amorphous substances, mainly composed of feldspar minerals; The particle size distribution of the raw material was tested using a laser particle size analyzer, and the results are as follows:Figure 2As shown, the sorting of volcanic ash raw materials is poor, and the particle size distribution is not concentrated, with a median particle size of 10.20 μ m. The specific surface area of volcanic ash was measured to be 2.4702 m · g using a physical adsorption instrument-1The bulk density was measured to be 1.674 7 g · cm by mercury intrusion test-3The chemical composition was determined by X-ray Fluorescence (XRF) spectroscopy, and the results expressed as oxides are as followsTable 1As shown, the overall content of silicon oxide and aluminum oxide in volcanic ash is relatively high, which meets the conditions for geopolymerization reaction. The alkaline activator is selected as NaOH solution, which is prepared by mixing 99% pure analytical sodium hydroxide provided by Beijing Chemical Plant with self-made distilled water. The surfactant is selected as Sika 540P polycarboxylate water reducer, purchased from Shanghai Chenqi Chemical Technology Co., Ltd.
| 种类 | SiO2 | FeO | Al2O3 | CaO | Na2O | K2O | MgO | TiO2 | P2O5 | MnO |
| 含量/% | 43.3 | 16.7 | 16.5 | 8.8 | 3.8 | 3.3 | 3.0 | 2.9 | 0.7 | 0.3 |
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To investigate the influence of the presence and types of functional groups in functionalized MWCNTs on the reinforcement effect of geopolymers, three commonly used MWCNTs were selected, namely raw MWCNTs, carboxylated MWCNTs, and hydroxylated MWCNTs, all purchased from Jiangsu Xianfeng Nanomaterials Technology Co., Ltd. There is no difference in their structural forms, with diameters ranging from 30 to 50 nm, lengths less than 10 μ m, and purities greater than 95%. The number of carboxyl and hydroxyl groups grafted varies, with carboxylated MWCNTs having a mass content of 0.73% and hydroxylated MWCNTs having a mass content of 1.06%.
| 试验组 | MWCNTs种类 | 质量掺量/% | 混合顺序 |
| P0 | 原始 | 0.00 | 先加MWCNTs分散液，再加NaOH溶液 |
| P05 | 原始 | 0.05 | 先加MWCNTs分散液，再加NaOH溶液 |
| P1 | 原始 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| P15 | 原始 | 0.15 | 先加MWCNTs分散液，再加NaOH溶液 |
| C1 | 羧基化 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| H1 | 羟基化 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| P1-2 | 原始 | 0.10 | 加MWCNTs与NaOH的混合溶液 |
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This article compares the effect of different ultrasound treatment durations on the dispersion of MWCNTs through microscopic observation and image processing. After obtaining MWCNTs dispersion solutions with different ultrasonic treatment durations, the MWCNTs dispersion solution was dropped onto a glass slide using a dropper, covered with a cover glass, and placed on the Keyence VR-3200 measuring instrument test bench. After about 5 minutes of image stabilization, microscopic images were taken at a magnification of 160 ×. 30 images were randomly taken for each group of dispersion solutions. Then, based on OpenCV's maximum inter class variance method, the image was binarized, and connected domain analysis was performed using seed filling method to obtain information on the number and area of aggregates in the image, in order to quantitatively evaluate the dispersion effect of MWCNTs.
Pour the freshly mixed geopolymer slurry directly into a stainless steel triple mold with dimensions of 40 mm × 40 mm × 160 mm, and vibrate it on a vibration table to remove bubbles. Wrap it with plastic film and place it in an oven at a temperature of 60 ℃ to cure for 6 hours. After demolding, continue to cure it in a curing box at a temperature of 60 ℃ and a relative humidity of 80% for 7 and 28 days until testing.
Table 3Summarized the calculation results related to aggregate area. In the dispersion without ultrasonic treatment, the area of aggregates accounted for 7.61% of the entire image proportion. After 15 minutes of ultrasonic treatment, it decreased to 2.31%, and after 30 minutes, it decreased to 1.87%. After 45 minutes, it was already below 1.00%. 15. The average aggregate area of the 30, 45, and 60 minute ultrasound groups decreased by 70%, 76%, 88%, and 93%, respectively, compared to the untreated dispersion. The maximum aggregate area increased from approximately 25000 μ m2Reduce to a final size of approximately 2200 μ m2It can be seen that MWCNTs dispersion with only surface active agents still contains a large number of aggregates, while ultrasonic treatment has a significant effect on achieving uniform dispersion. At the same time, the duration of ultrasonic treatment will significantly affect the dispersion effect of MWCNTs. The longer the ultrasonic treatment time, the greater the ultrasonic energy, and the better the dispersion effect. However, some scholars have suggested that higher ultrasound energy may damage the structure of MWCNTs, causing fiber fracture and reducing the aspect ratio of nanofibers, ultimately leading to a decrease in the efficiency of fiber load transmission and limited reinforcement effect[33]Therefore, the ultrasonic treatment time should not be too long. In this article, after 45 minutes of ultrasonic treatment, the range of 0-100 μ m2The proportion of aggregates has exceeded 85%, the proportion of aggregate area to image area is less than 1%, and the average aggregate area is less than 50 μ m2Therefore, it is believed that MWCNTs have achieved uniform dispersion after 45 minutes of ultrasonic treatment. The duration of ultrasound treatment for subsequent experiments in this article is uniformly 45 minutes.
| 超声处理时长/min | 团聚体面积占比/% | 平均团聚体面积/μm2 | 最大团聚体面积/μm2 |
| 0 | 7.61 | 650 | 24 727 |
| 15 | 2.31 | 153 | 3 227 |
| 30 | 1.87 | 79 | 2 365 |
| 45 | 0.86 | 46 | 2 242 |
| 60 | 0.53 | 31 | 2 231 |
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| 试验组 | 塌落度/mm | 塌落扩展度/mm |
| P0 | 113 | 201 |
| P05 | 110 | 198 |
| P1 | 106 | 195 |
| P15 | 88 | 183 |
| C1 | 107 | 196 |
| H1 | 111 | 199 |
| P1-2 | 35 |
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The flexural strength of geopolymer was tested at 7 and 28 days of curing, and the results are as follows:Figure 5As shown. Due to the fast solidification rate of the spherical particles formed during the preparation process of P1-2, it is difficult to form a uniform block when loaded into the mold. Therefore, mechanical performance testing was not conducted on this group.
For different types of MWCNTs test groups P1, C1, H1, the 7-day flexural strength results were similar, with values of 2.9, 3.0, and 3.0 MPa, respectively. Compared with the reference group's 2.4 MPa, these values increased by 20.8%, 25.0%, and 25.0%, respectively; At 28 days, the flexural strength still showed little difference, with values of 3.6, 3.7, and 3.8 MPa, respectively, which were 24.1%, 27.6%, and 31.0% higher than the reference group. It can be seen that different types of MWCNTs have an enhancing effect on the flexural strength of geopolymers, and functionalized MWCNTs have a superior effect. The reason for this may be that carboxyl and hydroxyl groups enhance the bonding between fibers and matrix interfaces from both physical and chemical perspectives, effectively exerting the mechanism of microcrack bridging[37].
To investigate the microstructure and reinforcement mechanism of MWCNTs in geopolymers, the 28 day old geopolymers were microscopically characterized. Scanning Electron Microscope (SEM) images of different experimental groups of geopolymers were taken as follows:Figure 7As shown. followFigure 7 (a)It can be seen that the gel generated by geopolymer reaction is relatively uniform and dense; causeFigure 7 (b)and(c)It can be seen that the fibers appear in the form of single strands without obvious entanglement or agglomeration, indicating that the dispersion effect remains good; At the same time, it can be found that the original MWCNTs have good compatibility with geopolymers and can be embedded into geopolymer products, playing a role in bridging microcracks and filling pores. in compliance withFigure 8As shown, the development of cracks in geopolymers can be divided into three stages, namely micro crack initiation, crack merging and propagation, and material failure stage[41]In the first stage, due to the bridging effect, MWCNTs effectively transferred the load between the geopolymer gel, which hindered the combination of cracks and the expansion of size, and could consume more energy before reaching the second stage. Therefore, the flexural strength of the geopolymer was improved; The filling effect reduces the pore size of the material and correspondingly lowers the porosity, thus improving the compressive strength. Meanwhile, fromFigure 7 (c)It can be seen that when the MWCNTs content is high, they are more likely to gather together, and even affect the dense growth of geopolymer gel, resulting in defects and reducing the lifting effect[42]; byFigure 7 (d)and(e)It can be seen that carboxylated and hydroxylated MWCNTs are more closely combined with geopolymer, and the fiber no longer has a smooth surface, but is coated by geopolymer gel, which indicates that MWCNTs become the core of geopolymer reaction and promote the growth of gel[43]This phenomenon indicates that the presence of carboxyl and hydroxyl groups forms more chemical interactions, strengthening the adhesion between MWCNTs and geopolymers, thereby making their strengthening effect more pronounced. This result corresponds to the strength enhancement effect; causeFigure 7 (f)It can be seen that MWCNTs appear in the form of large aggregates, indicating that the preparation method of the corresponding geopolymer in the P1-2 experimental group is prone to causing a large amount of MWCNTs aggregation; In fact, the dispersion effect of MWCNTs is directly related to the viscous state of the mixed solution, and the higher the viscosity, the worse the dispersion effect[44]At the same time, it also affects the preparation of geopolymer and cannot form a flowable slurry.
| 试验组 | 累计进汞量/ (mL·g-1) | 平均孔径/ nm | 2~50 nm孔隙占比/% | 大于50 nm孔隙占比/% | 孔隙率/ % |
| P0 | 0.1230 | 48.67 | 5.12 | 15.57 | 20.87 |
| P1 | 0.1152 | 47.76 | 5.02 | 15.05 | 20.07 |
| C1 | 0.1089 | 30.60 | 6.87 | 11.58 | 18.45 |
| H1 | 0.0949 | 27.71 | 6.28 | 12.12 | 18.40 |
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(2) The dosage, type, and mixing order of MWCNTs have varying degrees of influence on the viscosity of geopolymer slurries. When the dosage is 0.05% and 0.10%, MWCNTs have little effect on the slump and slump expansion of geopolymer slurry, and slightly decrease at 0.15%; Functionalized MWCNTs have improved hydrophilicity due to the presence of functional groups, which is beneficial for maintaining the slump and slump expansion of the slurry. Therefore, the viscosity remains basically unchanged; The mixing sequence of materials has a significant impact on the properties of geopolymers. Directly adding a mixed solution of MWCNTs and NaOH will cause volcanic ash to quickly bond and form spherical particles, and effective dispersion of fibers cannot be achieved. It is recommended to use the mixing sequence of adding MWCNTs dispersion first and then adding NaOH solution.
(3) MWCNTs can effectively enhance the flexural strength and compressive strength of geopolymers. For the original MWCNTs, the best improvement effect is achieved at a dosage of 0.10%, with a 24.1% and 13.2% increase in flexural and compressive strength, respectively, at 28 days; The functional groups of MWCNTs increase the wettability of fibers and enhance the chemical interaction between fibers and the geopolymer matrix, with a slightly better improvement effect than the original MWCNTs. The 28 day flexural and compressive strength of 0.10% carboxylated MWCNTs geopolymer increased by 27.6% and 14.3%, respectively, while hydroxylated MWCNTs increased by 31.0% and 15.9%, respectively.
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Figures(11) / Tables(5)
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LI Feng, ZHANG Rong-rong, ZHOU Si-qi, YANG Zhan-ning. Preparation and characterization of carbon nanotubes reinforced volcanic ash-based geopolymer[J]. Journal of Traffic and Transportation Engineering, 2023, 23(2): 153-165. doi: 10.19818/j.cnki.1671-1637.2023.02.011
| 种类 | SiO2 | FeO | Al2O3 | CaO | Na2O | K2O | MgO | TiO2 | P2O5 | MnO |
| 含量/% | 43.3 | 16.7 | 16.5 | 8.8 | 3.8 | 3.3 | 3.0 | 2.9 | 0.7 | 0.3 |
DownLoad:
CSV
| 试验组 | MWCNTs种类 | 质量掺量/% | 混合顺序 |
| P0 | 原始 | 0.00 | 先加MWCNTs分散液，再加NaOH溶液 |
| P05 | 原始 | 0.05 | 先加MWCNTs分散液，再加NaOH溶液 |
| P1 | 原始 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| P15 | 原始 | 0.15 | 先加MWCNTs分散液，再加NaOH溶液 |
| C1 | 羧基化 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| H1 | 羟基化 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| P1-2 | 原始 | 0.10 | 加MWCNTs与NaOH的混合溶液 |
DownLoad:
CSV
| 超声处理时长/min | 团聚体面积占比/% | 平均团聚体面积/μm2 | 最大团聚体面积/μm2 |
| 0 | 7.61 | 650 | 24 727 |
| 15 | 2.31 | 153 | 3 227 |
| 30 | 1.87 | 79 | 2 365 |
| 45 | 0.86 | 46 | 2 242 |
| 60 | 0.53 | 31 | 2 231 |
DownLoad:
CSV
| 试验组 | 塌落度/mm | 塌落扩展度/mm |
| P0 | 113 | 201 |
| P05 | 110 | 198 |
| P1 | 106 | 195 |
| P15 | 88 | 183 |
| C1 | 107 | 196 |
| H1 | 111 | 199 |
| P1-2 | 35 |
DownLoad:
CSV
| 试验组 | 累计进汞量/ (mL·g-1) | 平均孔径/ nm | 2~50 nm孔隙占比/% | 大于50 nm孔隙占比/% | 孔隙率/ % |
| P0 | 0.1230 | 48.67 | 5.12 | 15.57 | 20.87 |
| P1 | 0.1152 | 47.76 | 5.02 | 15.05 | 20.07 |
| C1 | 0.1089 | 30.60 | 6.87 | 11.58 | 18.45 |
| H1 | 0.0949 | 27.71 | 6.28 | 12.12 | 18.40 |
DownLoad:
CSV
| 种类 | SiO2 | FeO | Al2O3 | CaO | Na2O | K2O | MgO | TiO2 | P2O5 | MnO |
| 含量/% | 43.3 | 16.7 | 16.5 | 8.8 | 3.8 | 3.3 | 3.0 | 2.9 | 0.7 | 0.3 |
| 试验组 | MWCNTs种类 | 质量掺量/% | 混合顺序 |
| P0 | 原始 | 0.00 | 先加MWCNTs分散液，再加NaOH溶液 |
| P05 | 原始 | 0.05 | 先加MWCNTs分散液，再加NaOH溶液 |
| P1 | 原始 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| P15 | 原始 | 0.15 | 先加MWCNTs分散液，再加NaOH溶液 |
| C1 | 羧基化 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| H1 | 羟基化 | 0.10 | 先加MWCNTs分散液，再加NaOH溶液 |
| P1-2 | 原始 | 0.10 | 加MWCNTs与NaOH的混合溶液 |
| 超声处理时长/min | 团聚体面积占比/% | 平均团聚体面积/μm2 | 最大团聚体面积/μm2 |
| 0 | 7.61 | 650 | 24 727 |
| 15 | 2.31 | 153 | 3 227 |
| 30 | 1.87 | 79 | 2 365 |
| 45 | 0.86 | 46 | 2 242 |
| 60 | 0.53 | 31 | 2 231 |
| 试验组 | 塌落度/mm | 塌落扩展度/mm |
| P0 | 113 | 201 |
| P05 | 110 | 198 |
| P1 | 106 | 195 |
| P15 | 88 | 183 |
| C1 | 107 | 196 |
| H1 | 111 | 199 |
| P1-2 | 35 |
| 试验组 | 累计进汞量/ (mL·g-1) | 平均孔径/ nm | 2~50 nm孔隙占比/% | 大于50 nm孔隙占比/% | 孔隙率/ % |
| P0 | 0.1230 | 48.67 | 5.12 | 15.57 | 20.87 |
| P1 | 0.1152 | 47.76 | 5.02 | 15.05 | 20.07 |
| C1 | 0.1089 | 30.60 | 6.87 | 11.58 | 18.45 |
| H1 | 0.0949 | 27.71 | 6.28 | 12.12 | 18.40 |
DownLoad:
DownLoad:
