Microstructural Analysis and Synthesis of Organic Geopolymer Matrix | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Microstructural Analysis and Synthesis of Organic Geopolymer Matrix Iynthezhuthon Krishnamoorthy, LR Ganapathy Subramanian This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-4630110/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract Organic polymer resins generally cannot withstand temperatures exceeding 300°C, making them non-fire-resistant. However, inorganic alumino silicate polymers, synthesized by sodium silicate and sodium aluminate, have good thermal properties. This article discusses the synthesis of a geopolymer resin matrix based on different concentration ratios. The compositions of various constituent elements for the geopolymer matrix were varied, and hardeners were added with liquid solutions. The primary materials used are liquid sodium aluminate solution and sodium silicate solution, which are mixed with smaller quantities of fly ash and metakaolin. Several samples of geopolymer matrix were prepared and cured at elevated temperatures to remove water content. There was minimal shrinkage during curing. Microstructural tests were conducted to confirm the formation of a viable geopolymer resin, and the results confirmed the successful development of the geopolymer. Alkali activated material Fourier Transform Infrared Spectroscopy Geopolymer Inorganic polymers Microstructure Silicates Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Figure 14 INTRODUCTION Inorganic geopolymers are primarily composed of ceramics that covalently combine to create long-range non-crystalline structures. It is usually discovered that a new restricting substance first presented by Davidovits in 1978 can be utilized, with a zeolite piece yet unique in its portrayal of the undefined microstructure. The benefits of geopolymers include their outstanding durability, excellent tensile strength, and resistance to chemical corrosion and fire [ 2 ]. Geopolymer materials have been viewed as alternatives to Ordinary Portland Cement (OPC) since the early 1980s, mainly because of their superior performance and minimal carbon dioxide emissions. Researchers have successfully created the geopolymer coating, and it has outstanding features that can be utilized as coatings for lightweight polystyrene boards for walls, roofs, and partitions. These characteristics include high strength, artificial aging resistance, high-temperature resistance, and superior processing performance [ 3 ]. Geopolymer source materials truncated as GSM and soluble/exceptionally essential initiating fluids are two principal elements of geopolymer shortened as GP. GSM depends on aluminium silicate, which is rich in silica (Si) and aluminium (Al); in this way, subordinate materials can be framed. i.e., rice husk, silica exhaust, red mud, slag, fly ash debris, and similar kinds from the GSM. Aqueous solutions containing reactive ingredients (potassium/sodium hydroxide, phosphoric acid, potassium/sodium silicates, etc.) can be mixed with alumino-silicate wastes such as metakaolin, fly ash, blast furnace slag, rice husk ash, etc., to produce geopolymers [ 5 ]. Geopolymer is a flexible binder studied by a few mainstream researchers, yet it can turn into a supportable reverberation with Portland concrete for structural building applications. It is the greatest possible binder material [ 7 ]. Its application in the aerospace business is yet to be investigated. In any case, to comprehend a few parts of this new material, it is also essential to consider the previously mentioned terminologies so that the data accessible in the different gatherings is effortlessly utilized. In this article, the most widely recognized term, "Geopolymer," is embraced to exhibit information and discussions. Metakaolin MK-750-based and silica-based geopolymer pitches are utilized to impregnate fibers to get geopolymer matrix-based fibre composites. These items are fireproof and heatproof; they discharge no smoke or poisonous vapor. They were tried and suggested by significant global organizations like the Federal Aviation Administration. FAA chose the carbon-geopolymer composite as the top contender for the heat-proof lodge process. Geopolymers have been employed recently to immobilize dangerous metals. Studies have demonstrated that alkali-activated municipal solid waste incinerated fly ash successfully reduced the leaching effects of numerous dangerous metals [ 8 ]. Geopolymers are appealing host materials to immobilize atomic waste because of their high ecological sturdiness and adaptability to changes in waste. GEOPOLYMER SYNTHESIS: - GEOPOLYMERIZATION The process of geopolymerization involves synthesizing geopolymers by combining relatively smaller molecules into covalent bond chains. Several scientific experimental methods are used to carry out the geopolymerization reaction successfully, providing a detailed explanation of converting liquid Sodium Aluminate and Sodium Silicate precursors into geopolymers. An important distinction in the synthesis of geopolymer resin in this work is the use of both precursors in liquid form. Based on a literature survey, it is evident that considerable work is needed to formulate a viable geopolymer from two liquid sources. The process begins with the synthesis of geopolymer resin using titration. The burette is filled with Sodium Aluminate solution (NaAlO2), and the flask with Sodium Silicate solution (Na2SiO4). Titration is carried out with different ratios, adding drops every 10–20 seconds. Fly ash and Metakaolin powder are added as seeders to initiate the geopolymerization reaction. It is crucial to add sodium aluminate to sodium silicate slowly, similar to gradually diluting water with acid. Adding too much Sodium aluminate to the silicate solution at a rapid rate will cause the aluminate to precipitate out of the liquid solution. METHODOLOGY The initial step involves considering the ratio of Sodium Aluminate (NaAlO2) and Sodium Silicate (𝑁𝑎2𝑆𝑖𝑂4) solution. Take the appropriate volume of Na Si in a beaker and heat it on the hot plate magnetic stirrer until the solution reaches a temperature of 90–100 degrees Celsius. Then, add fly ash and a few milligrams of metakaolin (seeder), and use the magnetic stirrer to mix it evenly. Sodium aluminate should be titrated by adding it in drops every 10 seconds. Record the time taken to reach the required temperature of 90 to 100 degrees Celsius. Once the titration is complete and the required ratio is achieved, transfer the prepared resin into a mold for cooling. Allow the sample to set at room temperature for 24 hours, followed by curing in an oven at a maximum of 80 degrees Celsius for another 24 hours. The cured samples should then undergo FTIR (Fourier Transform Infrared spectroscopy) tests to verify whether the Geopolymerisation has occurred and to confirm the formation of geopolymer. SAMPLE DATA Several sample batches were prepared to determine the optimal ratio for synthesizing the geopolymer resin. The percentages that yielded the best results in each batch were chosen for the next round of testing to establish the best ratio for consistently producing a geopolymer matrix with reliable repeatability. Table.1 Sample Preparation with Different Ratios. Sample No. Concentration Ratio Seeder Used Titration Initial Temperature 1 1.5 (Si: Al = 60:40) Fly Ash 1gm 100 o C 2 2 (Si: Al = 40:20) Fly Ash 0.4 gm 80 o C 3 1.5 (Si: Al = 30:20) Fly Ash 0.3 gm 75 o C 4 2.5 (Si: Al = 80:32) Fly Ash 0.6 gm 76 o C 5 1.4 (Si: Al = 50:34) Metakaolin 0.3 gm 70 o C 6 1 (Si: Al = 50:50) Metakaolin 0.3 gm 100 o C 7 1.5 (Si: Al = 50:32) Metakaolin 0.3 gm 90 o C 8 2 (Si: Al = 50:25) Metakaolin 0.3 gm 92 o C 9 1.5 (Si: Al = 40:27) Metakaolin 0.6 gm 73 o C 10 2.5 (Si: Al = 50:20) Metakaolin 0.3gm 80 o C 11 3 (Si: Al = 50:16) Metakaolin 0.3gm 90 o C The above samples were kept at room temperature for 1 day and cured for 4 hours at about 70 degrees Celsius Table.2 Batch − 2- Hardened Samples and concentration ratio Sample No Concentration Ratio Seeder used 1 1.5 (Si: Al = 60:40) Fly Ash 1gm 2 2 (Si: Al = 40:20) Fly Ash 0.4 g 3 1.5 (Si: Al = 30:20) Fly Ash 8 2 (Si: Al = 50:25) Metakaolin 0.3 gm 9 1.5 (Si: Al = 40: 27) Metakaolin 0.6 gm The results of the previous batch of samples indicate that samples 3, 2, 1, 8, and 9 became hard and underwent geopolymerization reaction. These samples were re-prepared using the same steps, but this time they were cured for 24 hours at 100°C. This process was intended to reduce the water content in the geopolymer resin and promote bonding in the crystal structure. Batch − 3 While curing the second set of samples, it was observed that some of the samples were overheated at a high curing temperature, resulting in the formation of cracks. However, Sample 8 (Fly ash seeder) and Sample 3 (Metakaolin seeder) had fully hardened. The two affected samples were re-prepared and cured for 24 hours at a maximum of 80 degrees Celsius. CURING THE SAMPLES The best mechanical properties are observed when the geopolymer samples are cured at around 70°C, considered the optimum curing temperature. The samples were cured at 70°C for 4 hours in a hot air oven, resulting in reduced moisture content and hardening of five samples. All samples were then tested using FTIR Spectroscopy to confirm the formation of geopolymer. The first batch of samples was cured at 70°C for 4 hours, while the second batch was cured at 100°C for 24 hours. In the first case, more samples hardened, despite higher moisture content. In the second case, most samples overheated, leading to cracking. It is understood that the optimal temperature for the curing of the geopolymer resin is 75–85 degrees, as seen from the results of the third and final batch, where geopolymer resin is formed in a pseudo-gel state and can be used for making laminates. QUALITATIVE MATERIAL QUALIFICATION The spectral data of existing geopolymer materials are in the range of 900–1400 cm-1. Therefore, the FTIR data for all the precursor materials and finished products were compared to check whether the Geopolymerisation reaction had occurred, as described in the figures below. SAMPLE REQUIREMENT Various types of materials and instruments are used, and the requirements for the samples depend on them individually. As mentioned earlier, the samples being used can be in any form of matter. There is no restriction on the state of the sample. The area for the analysis could be as small as 8–12µm, so a microscopic attachment is included on the spectroscope. The wavelength for the geopolymer material is between 900–1400 cm^-1. The precursors used are: - Sodium Silicate - Sodium Aluminate - Fly Ash - Metakaolin powder The FTIR tests for each of these precursors have been done along with the prepared resins so that precise data about these precursors could be achieved, which are given below: RESULTS The different batches of the resins were synthesized. The samples were cured under a constant temperature environment as well. The samples were given for Fourier Mass Spectroscopy, and the results were collected. From the graph of the Spectroscopy, it's understood that the geopolymer signatures were found. The Geopolymer signature was found in the 900 cm-1 to 1300 cm-1 range. The samples were tested under the range of 400 cm – 4000 cm-1. The finding of each sample is explained as follows. BATCH – 2 SAMPLE -1 BATCH 2 SAMPLE - 2 BATCH 2 SAMPLE - 3 BATCH 2 SAMPLE- 8 BATCH 2 SAMPLE – 9 BATCH - 3 SAMPLE –8 BATCH 3 SAMPLE -3 CONCLUSION Geopolymers are inorganic materials that can be used to create a cost-effective matrix for composite materials. The resin can be made from inexpensive and readily available precursors such as sodium aluminate and sodium silicate solution. A significant discovery was made when a viable geopolymer resin was synthesized using two liquid-state precursors, unlike the conventional method used for concrete and civil applications. The most successful results for a geopolymer resin were found using fly ash with concentration ratios of sodium silicate to sodium aluminate at 30:20, and metakaolin with concentration ratios of sodium silicate to sodium aluminate at 50:25. Significant changes in the reaction occurred when the precursors were heated to a specific temperature during the preparation of samples, leading to a substantial increase in the rate of reaction of geopolymers. Declarations Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. References Aswani E, Lathi Karthi (2017) “A Literature Review on Fiber Reinforced Geopolymer Concrete” International Journal of Scientific & Engineering Research, Volume 8, Issue 2, ISSN 2229-5518 Shill, S.K., Al-Deen, S., Ashraf, M., et al., 2020. Resistance of fly ash based geopolymer mortar to both chemicals and high thermal cycles simultaneously. Construction and Building Materials 239, 117886. Abdel-Ghani, N.T., Elsayed, H.A., AbdelMoied, S., 2019. Geopolymer synthesis by the alkali-activation of blastfurnace steel slag and its fire-resistance. HBRC Journal 14 (2), 159e164. Davidovits.J(1991), ‘Geopolymers- inorganic polymeric new materials’, Journal thermal analysis, 37, pp.1633-1756 J.L. Provis, J.S.J. van Deventer, Geopolymers: Structure, Processing, Properties and Industrial Applications, 2009, ISBN 978-1-4398-0970-9. Davidovits.J and Davidovics.M(1991), “Geopolymer-ultra high temperature tooling material for the manufacture of advanced composite”, Proc.36th Int’l SAMPLE Symposium, pp 1939- 1949. Abdel-Gawwad H, Abo-El-Enein S. A novel method to produce dry geopolymer cement powder. HBRC J 2016;12(1):13–24. Liu, J., Hu, L., Tang, L., et al., 2020. Utilisation of municipal solid waste incinerator (MSWI) fly ash with metakaolin for preparation of alkali-activated cementitious material. Journal of Hazardous Materials 402, 123451. Ioanna Giannopoulou, Dimitrios Panias (2007)” Structure, Design and Applications of Geopolymeric Materials” Conference Paper https://www.researchgate.net/publication/234107877 J.A. Hammell, P.N. Balaguru, R.E. Lyon. (2000) “Strength retention of fire-resistant aluminosilicate–carbon composites under wet–dry conditions”, Composites: Part B 31 107–111 Mo Bing-hui, He Zhu, Cui Xue-min ⁎, He Yan, Gong Si-yu. (2014) “Effect of curing temperature on Geopolymerisation of metakaolin-based geopolymers” School of Chemistry and Chemical Engineering, Guangxi Key Lab of Petrochemical Resource Processing and Process Intensification Technology. M.S. Muñiz-Villarreal a, ⁎, A. Manzano-Ramírez a, S. Sampieri-Bulbarela a, J. Ramón Gasca-Tirado a, J.L. Reyes-Araiza a, J.C. Rubio-Ávalos a (2011). “The effect of temperature on the geopolymerization process of a metakaolin-based geopolymer”. Elsevier B.V. M. Arnoulta,b, M. Perronnetb, A. Autefb, S. Rossignola, (2018) ‘’How to control the geopolymer setting time with the alkaline silicate solution Journal of NonCrystalline Solids’’ · Chem. Rev. 47, 777-780. Nur Ain Jaya1, Mohd Mustafa Al Bakri Abdullah1, Long-yuan Li3, Andrei Victor Sandu, (2017) “Durability of Metakaolin Geopolymers with Various Sodium Silicate/Sodium Hydroxide Ratios against Sea water Exposure’’ Conference Paper in AIP Conference Proceedings · DOI: 10.1063/1.5003546 Navid Ranjbar, Mingzhong Zhang (2019). “Fiber reinforced geopolymer composites: A review” Article in Cement and Concrete Composites. DOI: 10.1016/j.cemconcomp. 103498 P. Balaguru, James Hammell, Richard E. Lyon, (1998), “Influence of reinforcement types on the flexural properties of geopolymer composites”, Article. Ralph Davidovits, Christine Pelegris, Joseph Davidovits, (2019), “Standardized Method in Testing Commercial Metakaolins for Geopolymer Formulations”, Technical Paper #26-MK-testing, Geopolymer Institute Library, ReenaAntil, Amit, Garvit, Ritesh, (2015), “Applications of Composite Materials in Aerospace” International journal of science technology and management. Sindhunata (2008), “A Conceptual Model of Geopolymerization”, Thesis for Doctor of Philosophy, Additional Declarations The authors declare no competing interests. Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. 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11","display":"","copyAsset":false,"role":"figure","size":187606,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eFig.10 Sample 8 FTIR Graph - Formation of Geopolymer at the peak of 943.98 cm\u003c/em\u003e\u003c/p\u003e","description":"","filename":"10.png","url":"https://assets-eu.researchsquare.com/files/rs-4630110/v1/58789f65b7bccdf13b15836f.png"},{"id":59014648,"identity":"48254e0d-549c-497c-8304-070162738115","added_by":"auto","created_at":"2024-06-25 10:07:34","extension":"png","order_by":12,"title":"Figure 12","display":"","copyAsset":false,"role":"figure","size":193872,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eFig 11 – Sample 9 – FTIR Graph - Formation of Geopolymer at the peak of 952.84 cm\u003c/em\u003e\u003c/p\u003e","description":"","filename":"11.png","url":"https://assets-eu.researchsquare.com/files/rs-4630110/v1/18c165fd29deaa7f0346e349.png"},{"id":59015104,"identity":"200bea0f-c413-4316-a9ef-ecf48fa9b69d","added_by":"auto","created_at":"2024-06-25 10:15:35","extension":"png","order_by":13,"title":"Figure 13","display":"","copyAsset":false,"role":"figure","size":153594,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eFig. 12- Sample 8 – FTIR Graph- Formation of Geopolymer at the peak of 962.48 cm\u003c/em\u003e\u003c/p\u003e","description":"","filename":"12.png","url":"https://assets-eu.researchsquare.com/files/rs-4630110/v1/322b6bde5d7990713ad40b9e.png"},{"id":59014653,"identity":"b1f9f04d-5060-4de9-820d-0538993a0690","added_by":"auto","created_at":"2024-06-25 10:07:36","extension":"png","order_by":14,"title":"Figure 14","display":"","copyAsset":false,"role":"figure","size":196218,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eFig.13 Sample- 3 – FTIR Graph- Formation of Geopolymer at the peak of 952.84 cm\u003c/em\u003e\u003c/p\u003e","description":"","filename":"13.png","url":"https://assets-eu.researchsquare.com/files/rs-4630110/v1/ae5cc55e385730591089225e.png"},{"id":59016009,"identity":"604334b8-7911-42b0-890e-07cfeeae7265","added_by":"auto","created_at":"2024-06-25 10:31:36","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":3525203,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4630110/v1/48f2c17e-092e-48e8-bae2-79fd9c9a5ebb.pdf"}],"financialInterests":"The authors declare no competing interests.","formattedTitle":"\u003cp\u003e\u003cstrong\u003eMicrostructural Analysis and Synthesis of Organic Geopolymer Matrix\u003c/strong\u003e\u003c/p\u003e","fulltext":[{"header":"INTRODUCTION","content":"\u003cp\u003eInorganic geopolymers are primarily composed of ceramics that covalently combine to create long-range non-crystalline structures. It is usually discovered that a new restricting substance first presented by Davidovits in 1978 can be utilized, with a zeolite piece yet unique in its portrayal of the undefined microstructure. The benefits of geopolymers include their outstanding durability, excellent tensile strength, and resistance to chemical corrosion and fire [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. Geopolymer materials have been viewed as alternatives to Ordinary Portland Cement (OPC) since the early 1980s, mainly because of their superior performance and minimal carbon dioxide emissions. Researchers have successfully created the geopolymer coating, and it has outstanding features that can be utilized as coatings for lightweight polystyrene boards for walls, roofs, and partitions. These characteristics include high strength, artificial aging resistance, high-temperature resistance, and superior processing performance [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. Geopolymer source materials truncated as GSM and soluble/exceptionally essential initiating fluids are two principal elements of geopolymer shortened as GP. GSM depends on aluminium silicate, which is rich in silica (Si) and aluminium (Al); in this way, subordinate materials can be framed. i.e., rice husk, silica exhaust, red mud, slag, fly ash debris, and similar kinds from the GSM. Aqueous solutions containing reactive ingredients (potassium/sodium hydroxide, phosphoric acid, potassium/sodium silicates, etc.) can be mixed with alumino-silicate wastes such as metakaolin, fly ash, blast furnace slag, rice husk ash, etc., to produce geopolymers [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. Geopolymer is a flexible binder studied by a few mainstream researchers, yet it can turn into a supportable reverberation with Portland concrete for structural building applications. It is the greatest possible binder material [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. Its application in the aerospace business is yet to be investigated. In any case, to comprehend a few parts of this new material, it is also essential to consider the previously mentioned terminologies so that the data accessible in the different gatherings is effortlessly utilized. In this article, the most widely recognized term, \"Geopolymer,\" is embraced to exhibit information and discussions. Metakaolin MK-750-based and silica-based geopolymer pitches are utilized to impregnate fibers to get geopolymer matrix-based fibre composites. These items are fireproof and heatproof; they discharge no smoke or poisonous vapor. They were tried and suggested by significant global organizations like the Federal Aviation Administration. FAA chose the carbon-geopolymer composite as the top contender for the heat-proof lodge process. Geopolymers have been employed recently to immobilize dangerous metals. Studies have demonstrated that alkali-activated municipal solid waste incinerated fly ash successfully reduced the leaching effects of numerous dangerous metals [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. Geopolymers are appealing host materials to immobilize atomic waste because of their high ecological sturdiness and adaptability to changes in waste.\u003c/p\u003e\n\u003ch3\u003eGEOPOLYMER SYNTHESIS: - GEOPOLYMERIZATION\u003c/h3\u003e\n\u003cp\u003eThe process of geopolymerization involves synthesizing geopolymers by combining relatively smaller molecules into covalent bond chains. Several scientific experimental methods are used to carry out the geopolymerization reaction successfully, providing a detailed explanation of converting liquid Sodium Aluminate and Sodium Silicate precursors into geopolymers. An important distinction in the synthesis of geopolymer resin in this work is the use of both precursors in liquid form. Based on a literature survey, it is evident that considerable work is needed to formulate a viable geopolymer from two liquid sources. The process begins with the synthesis of geopolymer resin using titration. The burette is filled with Sodium Aluminate solution (NaAlO2), and the flask with Sodium Silicate solution (Na2SiO4). Titration is carried out with different ratios, adding drops every 10\u0026ndash;20 seconds. Fly ash and Metakaolin powder are added as seeders to initiate the geopolymerization reaction. It is crucial to add sodium aluminate to sodium silicate slowly, similar to gradually diluting water with acid. Adding too much Sodium aluminate to the silicate solution at a rapid rate will cause the aluminate to precipitate out of the liquid solution.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e"},{"header":"METHODOLOGY","content":"\u003cp\u003eThe initial step involves considering the ratio of Sodium Aluminate (NaAlO2) and Sodium Silicate (𝑁𝑎2𝑆𝑖𝑂4) solution. Take the appropriate volume of Na Si in a beaker and heat it on the hot plate magnetic stirrer until the solution reaches a temperature of 90\u0026ndash;100 degrees Celsius. Then, add fly ash and a few milligrams of metakaolin (seeder), and use the magnetic stirrer to mix it evenly. Sodium aluminate should be titrated by adding it in drops every 10 seconds. Record the time taken to reach the required temperature of 90 to 100 degrees Celsius. Once the titration is complete and the required ratio is achieved, transfer the prepared resin into a mold for cooling. Allow the sample to set at room temperature for 24 hours, followed by curing in an oven at a maximum of 80 degrees Celsius for another 24 hours. The cured samples should then undergo FTIR (Fourier Transform Infrared spectroscopy) tests to verify whether the Geopolymerisation has occurred and to confirm the formation of geopolymer.\u003c/p\u003e\n\u003cdiv id=\"Sec4\" class=\"Section2\"\u003e\n \u003cp\u003eSAMPLE DATA\u003c/p\u003e\n \u003cp\u003eSeveral sample batches were prepared to determine the optimal ratio for synthesizing the geopolymer resin. The percentages that yielded the best results in each batch were chosen for the next round of testing to establish the best ratio for consistently producing a geopolymer matrix with reliable repeatability.\u003c/p\u003e\n \u003cp\u003e\u003cem\u003eTable.1 Sample Preparation with Different Ratios.\u003c/em\u003e\u003c/p\u003e\n \u003ctable id=\"Taba\" border=\"1\"\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSample No.\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eConcentration Ratio\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSeeder Used\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eTitration Initial Temperature\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;60:40)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash 1gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e100\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2 (Si: Al\u0026thinsp;=\u0026thinsp;40:20)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash 0.4 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e80\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;30:20)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash 0.3 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e75\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2.5 (Si: Al\u0026thinsp;=\u0026thinsp;80:32)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash 0.6 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e76\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.4 (Si: Al\u0026thinsp;=\u0026thinsp;50:34)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e70\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1 (Si: Al\u0026thinsp;=\u0026thinsp;50:50)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e100\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;50:32)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e90\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2 (Si: Al\u0026thinsp;=\u0026thinsp;50:25)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e92\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;40:27)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.6 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e73\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2.5 (Si: Al\u0026thinsp;=\u0026thinsp;50:20)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e80\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e11\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3 (Si: Al\u0026thinsp;=\u0026thinsp;50:16)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3gm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e90\u003csup\u003eo\u003c/sup\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003cp\u003e\u003c/p\u003e\n \u003cp\u003e\u003cem\u003eThe above samples were kept at room temperature for 1 day and cured for 4 hours at about 70 degrees Celsius\u003c/em\u003e\u003c/p\u003e\n \u003cp\u003e\u003cem\u003eTable.2 Batch \u0026minus;\u0026thinsp;2- Hardened Samples and concentration ratio\u003c/em\u003e\u003c/p\u003e\n \u003ctable id=\"Tabb\" border=\"1\"\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSample No\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eConcentration Ratio\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSeeder used\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;60:40)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash 1gm\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2 (Si: Al\u0026thinsp;=\u0026thinsp;40:20)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash 0.4 g\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;30:20)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eFly Ash\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2 (Si: Al\u0026thinsp;=\u0026thinsp;50:25)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.3 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.5 (Si: Al\u0026thinsp;=\u0026thinsp;40: 27)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMetakaolin 0.6 gm\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003cp\u003e\u003c/p\u003e\n \u003cp\u003eThe results of the previous batch of samples indicate that samples 3, 2, 1, 8, and 9 became hard and underwent geopolymerization reaction. These samples were re-prepared using the same steps, but this time they were cured for 24 hours at 100\u0026deg;C. This process was intended to reduce the water content in the geopolymer resin and promote bonding in the crystal structure.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec5\" class=\"Section2\"\u003e\n \u003cp\u003eBatch \u0026minus;\u0026thinsp;3\u003c/p\u003e\n \u003cp\u003eWhile curing the second set of samples, it was observed that some of the samples were overheated at a high curing temperature, resulting in the formation of cracks. However, Sample 8 (Fly ash seeder) and Sample 3 (Metakaolin seeder) had fully hardened. The two affected samples were re-prepared and cured for 24 hours at a maximum of 80 degrees Celsius.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec6\" class=\"Section2\"\u003e\n \u003cp\u003eCURING THE SAMPLES\u003c/p\u003e\n \u003cp\u003eThe best mechanical properties are observed when the geopolymer samples are cured at around 70\u0026deg;C, considered the optimum curing temperature. The samples were cured at 70\u0026deg;C for 4 hours in a hot air oven, resulting in reduced moisture content and hardening of five samples. All samples were then tested using FTIR Spectroscopy to confirm the formation of geopolymer. The first batch of samples was cured at 70\u0026deg;C for 4 hours, while the second batch was cured at 100\u0026deg;C for 24 hours. In the first case, more samples hardened, despite higher moisture content. In the second case, most samples overheated, leading to cracking.\u003c/p\u003e\n \u003cp\u003eIt is understood that the optimal temperature for the curing of the geopolymer resin is 75\u0026ndash;85 degrees, as seen from the results of the third and final batch, where geopolymer resin is formed in a pseudo-gel state and can be used for making laminates.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e\n \u003ch2\u003eQUALITATIVE MATERIAL QUALIFICATION\u003c/h2\u003e\n \u003cp\u003eThe spectral data of existing geopolymer materials are in the range of 900\u0026ndash;1400 cm-1. Therefore, the FTIR data for all the precursor materials and finished products were compared to check whether the Geopolymerisation reaction had occurred, as described in the figures below.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\n \u003cp\u003eSAMPLE REQUIREMENT\u003c/p\u003e\n \u003cp\u003eVarious types of materials and instruments are used, and the requirements for the samples depend on them individually. As mentioned earlier, the samples being used can be in any form of matter. There is no restriction on the state of the sample. The area for the analysis could be as small as 8\u0026ndash;12\u0026micro;m, so a microscopic attachment is included on the spectroscope. The wavelength for the geopolymer material is between 900\u0026ndash;1400 cm^-1.\u003c/p\u003e\n \u003cp\u003eThe precursors used are:\u003c/p\u003e\n \u003cp\u003e- Sodium Silicate\u003c/p\u003e\n \u003cp\u003e- Sodium Aluminate\u003c/p\u003e\n \u003cp\u003e- Fly Ash\u003c/p\u003e\n \u003cp\u003e- Metakaolin powder\u003c/p\u003e\n \u003cp\u003eThe FTIR tests for each of these precursors have been done along with the prepared resins so that precise data about these precursors could be achieved, which are given below:\u003c/p\u003e\n\u003c/div\u003e"},{"header":"RESULTS","content":"\u003cp\u003eThe different batches of the resins were synthesized. The samples were cured under a constant temperature environment as well. The samples were given for Fourier Mass Spectroscopy, and the results were collected. From the graph of the Spectroscopy, it\u0026apos;s understood that the geopolymer signatures were found. The Geopolymer signature was found in the 900 cm-1 to 1300 cm-1 range. The samples were tested under the range of 400 cm \u0026ndash; 4000 cm-1. The finding of each sample is explained as follows.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eBATCH \u0026ndash; 2 SAMPLE -1\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eBATCH 2\u0026nbsp;\u003c/strong\u003e\u003cstrong\u003eSAMPLE - 2\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eBATCH 2 SAMPLE - 3\u003c/p\u003e\n\u003cp\u003e\u0026nbsp;BATCH 2 SAMPLE- 8\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eBATCH 2 SAMPLE \u0026ndash; 9\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eBATCH - 3 SAMPLE \u0026ndash;8\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eBATCH 3\u0026nbsp;\u003c/strong\u003e\u003cstrong\u003eSAMPLE -3\u003c/strong\u003e\u003c/p\u003e"},{"header":"CONCLUSION","content":"\u003cp\u003eGeopolymers are inorganic materials that can be used to create a cost-effective matrix for composite materials. The resin can be made from inexpensive and readily available precursors such as sodium aluminate and sodium silicate solution. A significant discovery was made when a viable geopolymer resin was synthesized using two liquid-state precursors, unlike the conventional method used for concrete and civil applications. The most successful results for a geopolymer resin were found using fly ash with concentration ratios of sodium silicate to sodium aluminate at 30:20, and metakaolin with concentration ratios of sodium silicate to sodium aluminate at 50:25. Significant changes in the reaction occurred when the precursors were heated to a specific temperature during the preparation of samples, leading to a substantial increase in the rate of reaction of geopolymers.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eDeclaration of Competing Interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n \u003cli\u003eAswani E, Lathi Karthi (2017) \u0026ldquo;A Literature Review on Fiber Reinforced Geopolymer Concrete\u0026rdquo; International Journal of Scientific \u0026amp; Engineering Research, Volume 8, Issue 2, ISSN 2229-5518\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eShill, S.K., Al-Deen, S., Ashraf, M., et al., 2020. Resistance of fly ash based geopolymer mortar to both chemicals and high thermal cycles simultaneously. Construction and Building Materials 239, 117886.\u003c/li\u003e\n \u003cli\u003eAbdel-Ghani, N.T., Elsayed, H.A., AbdelMoied, S., 2019. Geopolymer synthesis by the alkali-activation of blastfurnace steel slag and its fire-resistance. HBRC Journal 14 (2), 159e164.\u003c/li\u003e\n \u003cli\u003eDavidovits.J(1991),\u0026nbsp;\u0026lsquo;Geopolymers- inorganic polymeric new materials\u0026rsquo;, Journal thermal analysis, 37, pp.1633-1756\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eJ.L. Provis, J.S.J. van Deventer, Geopolymers: Structure, Processing, Properties and Industrial Applications, 2009, ISBN 978-1-4398-0970-9.\u003c/li\u003e\n \u003cli\u003eDavidovits.J and Davidovics.M(1991),\u0026nbsp;\u0026ldquo;Geopolymer-ultra high temperature tooling material for the manufacture of advanced composite\u0026rdquo;, Proc.36th Int\u0026rsquo;l SAMPLE Symposium, pp 1939- 1949.\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eAbdel-Gawwad H, Abo-El-Enein S. A novel method to produce dry geopolymer cement powder. HBRC J 2016;12(1):13\u0026ndash;24.\u003c/li\u003e\n \u003cli\u003eLiu, J., Hu, L., Tang, L., et al., 2020. Utilisation of municipal solid waste incinerator (MSWI) fly ash with metakaolin for preparation of alkali-activated cementitious material. Journal of Hazardous Materials 402, 123451.\u003c/li\u003e\n \u003cli\u003eIoanna Giannopoulou, Dimitrios Panias\u0026nbsp;(2007)\u0026rdquo; Structure, Design and Applications of Geopolymeric Materials\u0026rdquo;\u0026nbsp;Conference Paper\u0026nbsp;https://www.researchgate.net/publication/234107877\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eJ.A. Hammell, P.N. Balaguru, R.E. Lyon.\u0026nbsp;(2000)\u0026nbsp;\u0026ldquo;Strength retention of fire-resistant aluminosilicate\u0026ndash;carbon composites under wet\u0026ndash;dry conditions\u0026rdquo;,\u0026nbsp;Composites: Part B 31 107\u0026ndash;111 \u0026nbsp;\u003c/li\u003e\n \u003cli\u003eMo Bing-hui, He Zhu, Cui Xue-min ⁎, He Yan, Gong Si-yu. (2014)\u0026nbsp;\u0026ldquo;Effect of curing temperature on Geopolymerisation of metakaolin-based geopolymers\u0026rdquo;\u0026nbsp;School of Chemistry and Chemical Engineering, Guangxi Key Lab of Petrochemical Resource Processing and Process Intensification Technology.\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eM.S. Mu\u0026ntilde;iz-Villarreal a, ⁎, A. Manzano-Ram\u0026iacute;rez a, S. Sampieri-Bulbarela a, J. Ram\u0026oacute;n Gasca-Tirado a, J.L. Reyes-Araiza a, J.C. Rubio-\u0026Aacute;valos a (2011). \u0026ldquo;The effect of temperature on the geopolymerization process of a metakaolin-based geopolymer\u0026rdquo;.\u0026nbsp;Elsevier B.V.\u003c/li\u003e\n \u003cli\u003eM. Arnoulta,b, M. Perronnetb, A. Autefb, S. Rossignola, (2018)\u0026nbsp;\u0026lsquo;\u0026rsquo;How to control the geopolymer setting time with the alkaline silicate solution Journal of NonCrystalline Solids\u0026rsquo;\u0026rsquo; \u0026middot;\u0026nbsp;Chem. Rev.\u0026nbsp;47, 777-780.\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eNur Ain Jaya1, Mohd Mustafa Al Bakri Abdullah1, Long-yuan Li3, Andrei Victor Sandu, (2017)\u0026nbsp;\u0026ldquo;Durability of Metakaolin Geopolymers with Various\u0026nbsp;Sodium Silicate/Sodium Hydroxide Ratios against Sea water Exposure\u0026rsquo;\u0026rsquo;\u0026nbsp;Conference Paper in AIP Conference Proceedings \u0026middot; DOI: 10.1063/1.5003546\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eNavid Ranjbar, Mingzhong Zhang (2019). \u0026ldquo;Fiber reinforced geopolymer composites: A review\u0026rdquo;\u0026nbsp;Article\u0026nbsp;in\u0026nbsp;Cement and Concrete Composites. DOI: 10.1016/j.cemconcomp. 103498\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eP. Balaguru, James Hammell, Richard E. Lyon, (1998),\u0026nbsp;\u0026ldquo;Influence of reinforcement types on the flexural properties of geopolymer composites\u0026rdquo;,\u0026nbsp;Article. \u0026nbsp;\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eRalph Davidovits, Christine Pelegris, Joseph Davidovits, (2019),\u0026nbsp;\u0026ldquo;Standardized Method in Testing Commercial Metakaolins for Geopolymer Formulations\u0026rdquo;,\u0026nbsp;Technical Paper #26-MK-testing, Geopolymer Institute Library, \u0026nbsp;\u003c/li\u003e\n \u003cli\u003eReenaAntil, Amit, Garvit, Ritesh, (2015), \u0026ldquo;Applications of Composite Materials in Aerospace\u0026rdquo; International journal of science technology and management. \u0026nbsp;\u0026nbsp;\u003c/li\u003e\n \u003cli\u003eSindhunata (2008), \u0026ldquo;A Conceptual Model of Geopolymerization\u0026rdquo;, Thesis for Doctor of Philosophy,\u0026nbsp;\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":true,"highlight":"","institution":"SRM Institute of Science and Technology","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"
[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Alkali activated material, Fourier Transform Infrared Spectroscopy, Geopolymer, Inorganic polymers, Microstructure, Silicates","lastPublishedDoi":"10.21203/rs.3.rs-4630110/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-4630110/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003e\u003cem\u003eOrganic polymer resins generally cannot withstand temperatures exceeding 300°C, making them non-fire-resistant. However, inorganic alumino silicate polymers, synthesized by sodium silicate and sodium aluminate, have good thermal properties. This article discusses the synthesis of a geopolymer resin matrix based on different concentration ratios. The compositions of various constituent elements for the geopolymer matrix were varied, and hardeners were added with liquid solutions. The primary materials used are liquid sodium aluminate solution and sodium silicate solution, which are mixed with smaller quantities of fly ash and metakaolin. Several samples of geopolymer matrix were prepared and cured at elevated temperatures to remove water content. There was minimal shrinkage during curing. Microstructural tests were conducted to confirm the formation of a viable geopolymer resin, and the results confirmed the successful development of the geopolymer.\u003c/em\u003e\u003c/p\u003e","manuscriptTitle":"Microstructural Analysis and Synthesis of Organic Geopolymer Matrix","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-06-25 10:07:29","doi":"10.21203/rs.3.rs-4630110/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"
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