Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
Revalorization of poorly reactive sources by mechanochemical activation: An alternative approach for sustainable cementitious binders
Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Structural and Fire Engineering.ORCID iD: 0000-0002-6797-9300
2022 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The latest report from the Intergovernmental Panel on Climate Change made once again clear the urge to take immediate actions to reduce the emissions of carbon dioxide and other greenhouse gases. Among the UN Sustainable Development Goals (SDGs), Nr. 12 (“Ensure sustainable consumption and production of raw materials”) aims to improve the industrial sector and to ensure a high quality of life. Concrete is the second most used material after water and in its traditional form utilizes cement clinker, whose production contributes to 8-10% of the anthropogenic CO2 emissions. Among the strategies to diminish the CO2 footprint, use of supplementary cementitious materials (SCM) and alkali-activated materials (AAM) are currently considered the most efficient countermeasures.  

Within this framework, revalorization of poorly reactive sources by mechanochemical activation can contribute to the development of novel binders with decreased CO2 footprint that can be utilized as partial or full replacement of Portland cement in concrete. Natural clays, mine tailings and air-cooled blast furnace slags (ACBFS), were activated in this study. Their applicability to be used in concretes as SCMs or/and AAMs was assessed. Natural clays are a mixture of various phases, whose compositions depends on weathering conditions. Naturally, they do not possess sufficient chemical reactivity to be utilized as SCMs. Similar properties possess mine tailings generated after extraction of precious elements, and slags produced in  blast furnaces of traditional steel plants.  

The present study aims to enhance the reactivity of these resources through mechanochemical activation (MCA) in a planetary ball mill. The process is considered a clean technology able to enhance the reactivity of crystalline materials without resorting to high processing temperatures or additional chemicals. MCA can induce amorphization, destroying the structure and breaking the bonds within the aluminosilicates and other minerals structure. The chosen parameters in the ball mill, as i.e. the filling amount, time of grinding, or speed of rotation, are strictly related to the degree of amorphization. Longer time of grinding, higher ball to processed powder (B/P) ratio, and higher grinding speeds generally increased the degree of the obtained amorphization. In such regard, an optimized process was chosen and further utilized to process all the poorly reactive resources. After MCA, the potential of clays and tailings as a SCM was investigated, while ACBFS was investigated as a precursor for alkali-activated materials. The achieved mechanical properties indicated a direct correlation between the enhanced amorphization degree of the mechanically activated clay and the increased strength values. The evaluation of SCMs was done by testing of their pozzolanic reactivity, enhanced after the mechanochemical activation. The reactivity was assessed by the strength activity index (SAI) and the Frattini test. Clays with higher content of clay minerals and tailings from the Kiruna mine deposit in Sweden showed increased pozzolanic reactivity and a great potential to be utilized as partial replacement of cement in concrete production. Furthermore, preliminary tests have shown that the alkali activation of the processed ACBFS produced solidified matrixes with considerable mechanical properties.   

Place, publisher, year, edition, pages
Luleå: Luleå University of Technology, 2022.
Series
Doctoral thesis / Luleå University of Technology, ISSN 1402-1544
Keywords [en]
clay, sustainability, mechanical activation, ball milling, supplementary cementitious materials, alkali-activated materials
National Category
Other Civil Engineering Other Materials Engineering
Research subject
Building Materials
Identifiers
URN: urn:nbn:se:ltu:diva-90365ISBN: 978-91-8048-081-9 (print)ISBN: 978-91-8048-082-6 (electronic)OAI: oai:DiVA.org:ltu-90365DiVA, id: diva2:1653435
Public defence
2022-06-17, F1031, Luleå, 10:00 (English)
Opponent
Supervisors
Available from: 2022-04-22 Created: 2022-04-21 Last updated: 2025-10-21Bibliographically approved
List of papers
1. Geopolymer Based on Mechanically Activated Air-cooled Blast Furnace Slag
Open this publication in new window or tab >>Geopolymer Based on Mechanically Activated Air-cooled Blast Furnace Slag
Show others...
2020 (English)In: Materials, E-ISSN 1996-1944, Vol. 13, no 5, article id 1134Article in journal (Refereed) Published
Abstract [en]

An efficient solution to increase the sustainability of building materials is to replace Portland cement with alkali-activated materials (AAM). Precursors for those systems are often based on water-cooled ground granulated blast furnace slags (GGBFS). Quenching of blast furnace slag can be done also by air but in that case, the final product is crystalline and with a very low reactivity. The present study aimed to evaluate the cementitious properties of a mechanically activated (MCA) air-cooled blast furnace slag (ACBFS) used as a precursor in sodium silicate alkali-activated systems. The unreactive ACBFS was processed in a planetary ball mill and its cementing performances were compared with an alkali-activated water-cooled GGBFS. Mixes based on mechanically activated ACBFS reached the 7-days compressive strength of 35 MPa and the 28-days compressive strength 45 MPa. The GGBFS-based samples showed generally higher compressive strength values.

Place, publisher, year, edition, pages
MDPI, 2020
Keywords
mechanochemistry, alkali activation, air-cooled slag, ground granulated slag, mechanical activation, cement-free mortars
National Category
Other Materials Engineering
Research subject
Building Materials
Identifiers
urn:nbn:se:ltu:diva-78303 (URN)10.3390/ma13051134 (DOI)000524060200112 ()32143319 (PubMedID)2-s2.0-85081681477 (Scopus ID)
Note

Validerad;2020;Nivå 2;2020-04-02 (alebob)

Available from: 2020-04-02 Created: 2020-04-02 Last updated: 2025-10-22Bibliographically approved
2. Activation of a Raw Clay by Mechanochemical Process: Effects of Various Parameters on the Process Efficiency and Cementitious Properties
Open this publication in new window or tab >>Activation of a Raw Clay by Mechanochemical Process: Effects of Various Parameters on the Process Efficiency and Cementitious Properties
2018 (English)In: Materials, E-ISSN 1996-1944, Vol. 11, no 10, article id 1860Article in journal (Refereed) Published
Abstract [en]

The efficiency of the mechanochemical activation (MCA) is influenced by various process parameters as well as by the properties of the treated material. The main objective of this research was to optimize the MCA process, gaining enhancement of the chemical reactivity of a Swedish raw clay, which is going to be used as an alkali-activated cementitious binder. The effects of the amount of water, the filling ratio, the rotation speed, and the grinding duration on the amorphization degree were evaluated by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). Generally, wet and dry processes showed an extensive amorphization of both kaolinite and muscovite minerals present in the studied clay. On the contrary, quartz was amorphized mainly by the wet grinding process. The efficiency of both dry and wet grinding processes was enhanced by the increased number of grinding media versus the amount of the activated material. However, longer processing times caused significant agglomeration while a higher rotational speed enhanced the amorphization. Preliminary tests have shown that alkali activation of the processed clays produced hardened samples. Furthermore, the increased amorphization corresponded to the increased compressive strength values.

Place, publisher, year, edition, pages
MDPI, 2018
Keywords
clay minerals, dry grinding, fine grinding, mechanochemical activation, mechanochemistry, wet grinding
National Category
Infrastructure Engineering
Research subject
Structural Engineering
Identifiers
urn:nbn:se:ltu:diva-71035 (URN)10.3390/ma11101860 (DOI)000448658400074 ()30274273 (PubMedID)2-s2.0-85054276282 (Scopus ID)
Note

Validerad;2018;Nivå 2;2018-10-03 (marisr)

Available from: 2018-09-30 Created: 2018-09-30 Last updated: 2025-10-22Bibliographically approved
3. Mechanochemically activated clay as asustainable cementitious binder
Open this publication in new window or tab >>Mechanochemically activated clay as asustainable cementitious binder
2019 (English)In: Proceedings ICSBM 2019: Volume - Greened Materials / [ed] V. Caprai; H.J.H. Brouwers, Technische Universiteit Eindhoven, 2019, Vol. 3, p. 462-468Conference paper, Published paper (Refereed)
Abstract [en]

High-temperature requirements, emission of hazardous substances from cement kilns and the significant CO2 footprint in the calcination step are factors requiring special attention in the cement industry. Local and commonly occurring clays can be a sustainable alternative for producing cementitious binders. Structural disorder in natural clay minerals can be induced through mechanochemical activation (MCA), by which the material develops an enhanced reactivity. The treatment of a Swedish natural clay through intensive grinding is carried out in order to assess its potential as a sustainable cementitious binder. Several grinding parameters influence a MCA product. The filling ratio of the jar, the rotation speed, the time of grinding, as well as wet and dry environment, are variated to optimize the MCA process. The MCA process doesnot require high temperatures or added chemicals and shorter processing times can avoid high-energy requirements during fine grinding. The structural changes of the clay were analysed by X-Ray Diffraction (XRD). Analysis of the particle size distribution of the raw and processed clay suggested a correlation with the grinding duration. An increased ratio of grinding media versus the amount of ground material, while longer grinding duration increased the overall efficiency of the MCA process. The strength activity index (SAI) indicated an enhanced pozzolanic activity for the mechanochemically processed clay. Compressive strength tests have shown a strong correlation between an enhanced amorphization rate and increased compressive strength values.

Place, publisher, year, edition, pages
Technische Universiteit Eindhoven, 2019
Keywords
alternative cementitious binders, mechanochemical activation, sustainable building materials, mechanochemistry, clay
National Category
Other Materials Engineering
Research subject
Building Materials
Identifiers
urn:nbn:se:ltu:diva-76601 (URN)
Conference
2nd International Conference of Sustainable Building Materials (ICSBM 2019), Eindhoven, The Netherlands, August 12-15, 2019
Funder
Swedish Research Council Formas
Available from: 2019-11-04 Created: 2019-11-04 Last updated: 2025-10-22Bibliographically approved
4. Optimization of the Process Parameters Controlling the Degree of Amorphization during Mechanical Activation of Clay Using the Taguchi Method
Open this publication in new window or tab >>Optimization of the Process Parameters Controlling the Degree of Amorphization during Mechanical Activation of Clay Using the Taguchi Method
2019 (English)In: The 1st International Conference on Smart Materials for Sustainable Construction, MDPI, 2019, article id 15Conference paper, Oral presentation with published abstract (Refereed)
Abstract [en]

Mechanical activation in a planetary ball mill (BM) is an environmentally friendly process able to enhance the chemical and pozzolanic activity of natural clays. Those materials can be used as supplementary cementitious materials (SCMs) to partially replace Portland cement in concrete. The process parameters of the BM are directly related to the degree of amorphization and thus to the enhancement of the chemical activity. Design of experiments (DOE) is a well-known statistical tool, which can assist in selecting optimized conditions and in obtaining systematic data. However, full factorial design requires a large number of experiment. Taguchi method is based on the use of an Orthogonal Array (OA) to evaluate optimization of the selected factors but with less required experiments. In this study, three factors, each on 2 levels, were selected: ball to powder ratio (B/P) with level 3 and 25, time of grinding with level 5 and 20, and water to powder ratio (W/P) with level 0 and 1. The degree of amorphization (DOA) was selected as the main response for the Taguchi method. DOA was calculated as the ratio between the integral intensities of the main peak of the kaolinite [001] before and after grinding. For dry grinding, the predicted optimized value of DOA complied with the experimental results. Maximized DOA value was achieved for B/P equal to 25 and the grinding duration of 20. This method can be a valuable tool to predict the amorphization degree of minerals present in the natural clay, leading to the optimization of the mechanical activation process.

Place, publisher, year, edition, pages
MDPI, 2019
Series
Proceedings, E-ISSN 2504-3900 ; 34(1)
Keywords
mechanical activation, degree of amorphization, Taguchi method, clay-based binder, sustainable building materials, ball mill
National Category
Building Technologies
Research subject
Building Materials
Identifiers
urn:nbn:se:ltu:diva-76737 (URN)10.3390/proceedings2019034015 (DOI)
Conference
1st International Conference on Smart Materials for Sustainable Construction (SMASCO 2019), Luleå, Sweden, December 10-12, 2019
Available from: 2019-11-18 Created: 2019-11-18 Last updated: 2025-10-22Bibliographically approved
5. Mechanochemical activation of natural clay minerals: an alternative to produce sustainable cementitious binders – review
Open this publication in new window or tab >>Mechanochemical activation of natural clay minerals: an alternative to produce sustainable cementitious binders – review
2019 (English)In: Mineralogy and Petrology, ISSN 0930-0708, E-ISSN 1438-1168, Vol. 113, no 4, p. 449-462Article in journal (Refereed) Published
Abstract [en]

Mechanochemical activation can be defined as a process able to induce structural disorder through intensive grinding. In certain conditions, it may increase the chemical reactivity of the processed material. The process is extensively utilized in extractive metallurgy, synthesis of nanocomposites or pharmacology. It is also considered an environmentally friendly alternative to activate kaolinitic clay avoiding high calcination temperature. This paper aims to give a comprehensive overview of the process, its evolution, process parameters and applications. The paper focuses on the mechanochemical treatment of natural clay minerals, aiming at their transformation into cementitious or pozzolanic materials. It provides a summarized review of the theories related to the mechanochemistry and discusses commonly used models. The paper also analyzes various key factors and parameters controlling the mechanochemical activation process. The optimization and control of the several factors, as the filling ratio, the grinding media, the velocity, the time of grinding, etc., can promote developments and new research opportunities on different fields of application. Examples of applications, with a special focus on mechanochemically activated clay minerals and their use as cementitious binders, are listed as well.

Place, publisher, year, edition, pages
Springer, 2019
Keywords
Mechanochemistry, Grinding, Mechanochemical activation, Clay minerals, Kaolin
National Category
Other Materials Engineering
Research subject
Building Materials
Identifiers
urn:nbn:se:ltu:diva-73879 (URN)10.1007/s00710-019-00666-y (DOI)000475666800002 ()2-s2.0-85065650673 (Scopus ID)
Note

Validerad;2019;Nivå 2;2019-07-12 (johcin)

Available from: 2019-05-08 Created: 2019-05-08 Last updated: 2025-10-22Bibliographically approved
6. Enhancement of the pozzolanic activity of natural clays by mechanochemical activation
Open this publication in new window or tab >>Enhancement of the pozzolanic activity of natural clays by mechanochemical activation
Show others...
2022 (English)In: Construction and Building Materials, ISSN 0950-0618, E-ISSN 1879-0526, Vol. 352, article id 128739Article in journal (Refereed) Published
Abstract [en]

Replacement of cement with supplementary cementitious materials (SCMs) is a proven method to reduce clinker in cement and contribute to decreased CO2 emissions. Natural clays are commonly occurring materials that do not possess pozzolanic activity in their original state. Mechanochemical activation (MCA) can be an alternative and sustainable method to enhance their reactivity. In this study, the pozzolanic reactivity of three natural clays, originating from Sweden, was analyzed after the application of MCA in a planetary ball mill. Strength activity index (SAI), Frattini test, and conductivity test were used to evaluate the pozzolanic reactivity. All processed clays by MCA have achieved a SAI greater than 100%, while the Frattini test indicated an improved pozzolanic activity of samples containing a higher amount of clay minerals. The obtained results show that MCA could improve the pozzolanic reactivity, but the effect depends on the mineralogical composition and particle size of the clays.

Place, publisher, year, edition, pages
Elsevier, 2022
Keywords
Grinding, Blended Cement, Pozzolan, SCMs, Clays
National Category
Other Civil Engineering Other Materials Engineering
Research subject
Building Materials
Identifiers
urn:nbn:se:ltu:diva-90356 (URN)10.1016/j.conbuildmat.2022.128739 (DOI)000933926800004 ()2-s2.0-85137668310 (Scopus ID)
Funder
Swedish Research Council Formas
Note

Validerad;2022;Nivå 2;2022-09-28 (hanlid)

Available from: 2022-04-21 Created: 2022-04-21 Last updated: 2025-10-21Bibliographically approved
7. Revalorization of mine tailings by mechanochemical activation
Open this publication in new window or tab >>Revalorization of mine tailings by mechanochemical activation
(English)Manuscript (preprint) (Other academic)
Keywords
mine tailings, mechanochemical activation, supplementary cementitious materials, pozzolanic activity, revalorization
National Category
Other Civil Engineering Other Materials Engineering
Research subject
Building Materials
Identifiers
urn:nbn:se:ltu:diva-90357 (URN)
Available from: 2022-04-21 Created: 2022-04-21 Last updated: 2025-10-21

Open Access in DiVA

fulltext(7393 kB)1435 downloads
File information
File name FULLTEXT01.pdfFile size 7393 kBChecksum SHA-512
b4363b78dba319ade1546ea2a3b3aba26380f11232c14e1da0410b8c362ffaaf8bc7c7269d6c58777bdd5081805f2411b2f19e63abca169150987ab8540447ec
Type fulltextMimetype application/pdf

Authority records

Tole, Ilda

Search in DiVA

By author/editor
Tole, Ilda
By organisation
Structural and Fire Engineering
Other Civil EngineeringOther Materials Engineering

Search outside of DiVA

GoogleGoogle Scholar
Total: 1438 downloads
The number of downloads is the sum of all downloads of full texts. It may include eg previous versions that are now no longer available

isbn
urn-nbn

Altmetric score

isbn
urn-nbn
Total: 1802 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf