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Cited by 12Concrete and Cement Materials ResearchZeolite Catalysis and SynthesisMagnesium Oxide Properties and Applications

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Formation of Geopolymers Using Sodium Silicate Solution and Aluminum Orthophosphate

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Partschefeld, Stephan, Wiegand, Torben, Bellmann, Frank, Osburg, Andrea·2020·Materials
DOI 10.3390/ma13184202PMC PMC7560488
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Abstract

This paper reports the formation and structure of fast setting geopolymers activated by using three sodium silicate solutions with different modules (1.6, 2.0 and 2.4) and a berlinite-type aluminum orthophosphate. By varying the concentration of the aluminum orthophosphate, different Si/Al-ratios were established (6, 3 and 2). Reaction kinetics of binders were determined by isothermal calorimetric measurements at 20 °C. X-ray diffraction analysis as well as nuclear magnetic resonance (NMR) measurements were performed on binders to determine differences in structure by varying the alkalinity of the sodium silicate solutions and the Si/Al-ratio. The calorimetric results indicated that the higher the alkalinity of the sodium silicate solution, the higher the solubility and degree of conversion of the aluminum orthophosphate. The results of X-ray diffraction and Rietveldt analysis, as well as the NMR measurements, confirmed the assumption of the calorimetric experiments that first the aluminum orthophosphate was dissolved and then a polycondensation to an amorphous aluminosilicate network occurred. The different amounts of amorphous phases formed as a function of the alkalinity of the sodium silicate solution, indicate that tetrahydroxoaluminate species were formed during the dissolution of the aluminum orthophosphate, which reduce the pH value. This led to no further dissolution of the aluminum orthophosphate, which remained unreacted.

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Crossref · 10.3390/ma13184202

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Figure 1 Static 29Si nuclear magnetic resonance (NMR) spectra of used silica solutions.
Figure 1 Static 29Si nuclear magnetic resonance (NMR) spectra of used silica solutions.CC BY · PubMed Central
Figure 2 Scanning electron microscopy (SEM) image of the used aluminum orthophosphate.
Figure 2 Scanning electron microscopy (SEM) image of the used aluminum orthophosphate.CC BY · PubMed Central
Figure 3 27Al MAS NMR spectrum (a) and the 31P MAS NMR spectrum (b) of the used AlPO4.
Figure 3 27Al MAS NMR spectrum (a) and the 31P MAS NMR spectrum (b) of the used AlPO4.CC BY · PubMed Central
Figure 4 Calorimetric measurements of the reaction kinetics of sodium silicate solution (module: 1.6) and different Si/Al-ratios of 2, 3 and 6.
Figure 4 Calorimetric measurements of the reaction kinetics of sodium silicate solution (module: 1.6) and different Si/Al-ratios of 2, 3 and 6.CC BY · PubMed Central
Figure 5 Calorimetric measurements of the reaction kinetics of sodium silicate solution (module: 2.0) and different Si/Al-ratios of 2, 3 and 6.
Figure 5 Calorimetric measurements of the reaction kinetics of sodium silicate solution (module: 2.0) and different Si/Al-ratios of 2, 3 and 6.CC BY · PubMed Central
Figure 6 Calorimetric measurements of the reaction kinetics of sodium silicate solution (module: 2.4) and different Si/Al-ratios of 2, 3 and 6.
Figure 6 Calorimetric measurements of the reaction kinetics of sodium silicate solution (module: 2.4) and different Si/Al-ratios of 2, 3 and 6.CC BY · PubMed Central
Figure 7 Phase composition of the formed geopolymer binders using a Si/Al-ratio of 6 and different sodium silicate solution (SiO2/Na2O = 1.6, 2.0 and 2.4).
Figure 7 Phase composition of the formed geopolymer binders using a Si/Al-ratio of 6 and different sodium silicate solution (SiO2/Na2O = 1.6, 2.0 and 2.4).CC BY · PubMed Central
Figure 8 Phase composition of the formed geopolymer binders using a Si/Al-ratio of 3 and different sodium silicate solution (SiO2/Na2O = 1.6, 2.0 and 2.4).
Figure 8 Phase composition of the formed geopolymer binders using a Si/Al-ratio of 3 and different sodium silicate solution (SiO2/Na2O = 1.6, 2.0 and 2.4).CC BY · PubMed Central
Figure 9 Phase composition of the formed geopolymer using a Si/Al-ratio of 2 and different sodium silicate solution (SiO2/Na2O = 1.6, 2.0 and 2.4).
Figure 9 Phase composition of the formed geopolymer using a Si/Al-ratio of 2 and different sodium silicate solution (SiO2/Na2O = 1.6, 2.0 and 2.4).CC BY · PubMed Central
Figure 10 Static 29Si NMR of silica solution (SiO2/Na2O = 2.4, 2.0 and 1.6, dotted lines) and 29Si MAS NMR of binders A-C (solid lines), formed by addition of berlinite (Si/Al = 3) to these solutions.
Figure 10 Static 29Si NMR of silica solution (SiO2/Na2O = 2.4, 2.0 and 1.6, dotted lines) and 29Si MAS NMR of binders A-C (solid lines), formed by addition of berlinite (Si/Al = 3) to these solutions.CC BY · PubMed Central
Figure 11 Static 29Si NMR of silica solution (SiO2/Na2O = 1.6, red dotted line) and 29Si MAS NMR of binders C-E, formed by addition of berlinite (Si/Al = 2, 3 and 6) to this solution.
Figure 11 Static 29Si NMR of silica solution (SiO2/Na2O = 1.6, red dotted line) and 29Si MAS NMR of binders C-E, formed by addition of berlinite (Si/Al = 2, 3 and 6) to this solution.CC BY · PubMed Central
Scheme 1 Dissolution reaction of berlinite under alkaline conditions.
Scheme 1 Dissolution reaction of berlinite under alkaline conditions.CC BY · PubMed Central
Figure 12 27Al MAS NMR spectra of binders A–E.
Figure 12 27Al MAS NMR spectra of binders A–E.CC BY · PubMed Central
Figure 13 31P MAS NMR spectra of binders A–E.
Figure 13 31P MAS NMR spectra of binders A–E.CC BY · PubMed Central

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Research works printed but not linked: 26

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Metadata

Authors
Partschefeld, S., Wiegand, T., Bellmann, F., & Osburg, A.
Affiliations
Bauhaus-Universität Weimar (DE)
Corresponding author
Partschefeld, Stephan
ORCID
Venue
Materials
Publisher
MDPI AG
Published
2020-09-21
Volume
13
Issue
18
Pages
4202
ISSN
1996-1944 (ISSN-L)
DOI
10.3390/ma13184202
PMC
PMC7560488
OpenAlex
W3087219239
Cited by
12
References
0
Citations by year
2026: 2 · 2025: 1 · 2024: 4 · 2023: 2 · 2022: 2 · 2021: 1
FWCI
0.73
Type
journal article
Language
en
Open access
Licence
Locations
  • Materials (publishedVersion, cc-by)
  • PubMed Central (publishedVersion, cc-by)
  • PubMed (publishedVersion)
  • DOAJ (DOAJ: Directory of Open Access Journals) (submittedVersion, cc-by-sa)
  • Publication Server of Weimar Bauhaus-University (Weimar Bauhaus-University) (submittedVersion, cc-by)
  • Common Library Network (Der Gemeinsame Bibliotheksverbund) (submittedVersion, cc-by)
Topics
  • Physical Sciences › Engineering › Civil and Structural Engineering › Concrete and Cement Materials Research
  • Physical Sciences › Chemistry › Inorganic Chemistry › Zeolite Catalysis and Synthesis
  • Physical Sciences › Materials Science › Materials Chemistry › Magnesium Oxide Properties and Applications
Keywords
geopolymer, sodium silicate solution, berlinite, Si/Al ratio, alkalinity, reaction kinetics, calorimetry, polycondensation, binder structure

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