Article(id=1320090055205573519, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320090049606172775, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20240678, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1729958400000, receivedDateStr=2024-10-27, revisedDate=1734883200000, revisedDateStr=2024-12-23, acceptedDate=null, acceptedDateStr=null, onlineDate=1792663595248, onlineDateStr=2026-10-22, pubDate=1747670400000, pubDateStr=2025-05-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792663595248, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792663595247, creator=13701087609, updateTime=1792663595247, updator=13701087609, issue=Issue{id=1320090049606172775, tenantId=1146029695717560320, journalId=1263187385517883426, year='2025', volume='53', issue='5', pageStart='1031', pageEnd='1402', issueExtLink='null', onlineDate='null', pubDate='1747670400000', pubDateStr='2025-05-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792663593913, creator='13701087609', updateTime=1792663765419, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320090769013190788, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320090049606172775, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320090769013190789, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320090049606172775, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1205, endPage=1213, ext={EN=ArticleExt(id=1320090056115737489, articleId=1320090055205573519, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Influence of Aluminum Salts on Properties and Hydration of Magnesium Potassium Phosphate Cements, columnId=1319726165087077079, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Article, runingTitle=null, highlight=null, articleAbstract=
Introduction Magnesium potassium phosphate (MKP) cements are normally composed of dead-burnt magnesia and monopotassium phosphate (KH2PO4), which react in water and yield the main hydrate of K-struvite (MgKPO4·6H2O). MKP cements have been frequently used as rapid repair materials in the field of civil engineering and as solidification/stabilization agents in the field of waste managements, due to the unique properties, such as fast setting, high early strength, low drying shrinkage, strong bonding to old Portland cement concrete substrates, low pH value, and so on. Boron compounds are the de facto standard retarders of MKP cements. Normally the increase of boron compound dosage could prolong MKP cement setting, but result in slower strength development, especially at early ages. Therefore, in order to obtain sufficient setting time and early strength at the same time, research attempts on seeking new retarders have been carrying out in recent years. Aluminum salts, Al(NO3)3 and Al2(SO4)3, were among those reported chemicals, showing promising retardation effect, especially at low M/P molar ratios. However, influence of aluminum salts on properties and hydration of MKP cements are yet to be explored, as several important aspects remain unclear, such as their impact differences on MKP cement early and late strengths, roles of Al3+ and of different anions on governing the hydration. Therefore, in this work influence of three common aluminum salts, AlCl3, Al(NO3)3 and Al2(SO4)3, on properties and hydration of MKP cements at magnesium-to-phosphate (M/P) molar ratio of 4 and water-to-cement (w/c) ratios of 0.27 and 5.00 was studied.
Methods The raw materials for the preparation of MKP cements were industrial-grade dead-burnt magnesia and KH2PO4. The chemicals in analytical grade were borax (Na2B4O7·10H2O), Al2(SO4)3·16H2O, Al(NO3)3·9H2O, and AlCl3·6H2O. The MKP cement pastes and suspensions were prepared at same M/P molar ratio of 4, and at w/c ratios of 0.27 and 5.00. The aluminum salts were dissolved in the portioned mixing water before use, and the Al concentrations for the pastes and the suspensions were 600 mmol/L and 32.4 mmol/L, respectively. For comparison purpose, borax was used as reference, of which the dosages were 5.15% and 6.08%, by weight of cement, equal to the dosages of Al2(SO4)3·16H2O and Al(NO3)3·9H2O, respectively. Vicat needle test was used to determine the paste final setting time. Flexural and compressive strengths of the pastes with the dimensions of 25 mm × 25 mm ×125 mm were measured after 1, 3 h, 1, 7, 28, 90 d and 400 d. Additional strength measurements were carried out after 6 h and 12 h for the paste with Al(NO3)3, due to the low strengths within the first 3 h. Hydration heat of the pastes up to 24 h was measured using an isothermal calorimeter (TAM) at 20 ℃, using internal mixing method. Moreover, hydrate assemblages of the pastes after 28 d and 400 d were analyzed using XRD, TGA and FTIR methods. To track the aqueous evolution, pH and electrical conductivity of the MKP cement suspensions were continuously monitored up to 24 h at 25 ℃. Also the aqueous compositions were determined using ion chromatography and inductively coupled plasma after 15, 33 min, 3 h, 1 d and 7 d.
Results and discussion Compared to the reference paste, the additions of Al2(SO4)3, Al(NO3)3 and AlCl3 could extend the setting time by around 2.5, 3.1 times and 5.1 times, respectively, corresponding to around 25%, 45% and 80% increases as compared to borax at 6.08%. It indicates better retardation effect of the aluminum salts and the anions taking effect in the order of Cl-, NO3-, and SO42-. In contrast to Al(NO3)3 and Al2(SO4)3, AlCl3 leads to clear sample expansion and cracks, suggesting its unsuitable use in MKP cement-based materials. Moreover, compared to the reference paste, both Al(NO3)3 and Al2(SO4)3 lower the early strengths. The strength weakening effect of Al2(SO4)3 mainly occur within the first 3 h, and of Al(NO3)3 is more pronounced and lasts longer up to around 12 h. However, thereafter, the strengths of the pastes with Al(NO3)3 and Al2(SO4)3 gain fast, leading consequently to similar or even slightly higher strengths at late ages compared to the reference paste.
Al(NO3)3 shows better effects on slowing down hydration heat release and on decreasing cumulative heat up to 24 h, compared to Al2(SO4)3, in agreement with the setting time results. Both Al(NO3)3 and Al2(SO4)3 do not change the main hydrate, which remains K-struvite, but slightly decrease the formation contents. Compared to Al2(SO4)3, Al(NO3)3 lowers more the system pH value and extends hydration stages to later reaction times, consistent with the results of setting time and calorimetry, revealing stronger effect of NO3- than SO42- under same Al3+ concentration. The aqueous composition results suggest well that Al3+ is precipitated rapidly at the beginning of reaction, leading to certain amorphous Al-containing phases. At low w/c of 0.27 the anions of NO3- and SO42- are precipitated as crystalline KNO3 and K2SO4, filling micro-pores in hardened paste matrices, which indicates attention required on matrix volume stability as high dosages of these aluminum salts are used.
Conclusions The main findings of this work are concluded as follows. All the investigated aluminum salts (AlCl3, Al(NO3)3 and Al2(SO4)3) could retard MKP cement setting. Furthermore, they show better retardation effect than borax at the same dosage. In contrast to Al(NO3)3 and Al2(SO4)3, AlCl3 could lead to sample expansion and cracks, indicating its unsuitable use in MKP cement-based materials. Moreover, both Al2(SO4)3 and Al(NO3)3 could lower the cement early strengths, which occurs within the first 3 h and 12 h, respectively, consistent with their retardation effects. But they show no adverse impacts on the paste strengths at late ages, compared to the reference paste. Compared to Al2(SO4)3, Al(NO3)3 is more effective on reducing system pH, extending hydration stage, slowing down hydration heat release, and on inhibiting slightly K-struvite precipitation, which contribute to better retardation effect. In addition to K-struvite, small contents of amorphous Al-containing hydrates and of crystalline KNO3 and K2SO4 are precipitated in the hydrated matrices, affecting the paste properties.
, authors=Biwan XU, Qiushi ZHANG, Yizhou ZHAO, authorsList=Biwan XU, Qiushi ZHANG, Yizhou ZHAO, authorCompany=null, correspAuthors=null, authorNote=
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铝盐能够延缓磷酸钾镁水泥凝结，但不同铝盐对其性能和水化的影响差异和机理尚未清晰。通过凝结时间测试、强度测试、水化热实验、X射线衍射、热重和Fourier红外光谱分析、pH值与电导率测试以及离子浓度测试实验研究了3种常见铝盐对磷酸钾镁水泥性能和水化的影响。结果表明：与等质量掺量的硼酸钠相比，AlCl3、Al（NO3）3和Al2（SO4）3作用下的净浆凝结时间可分别延长80%、45%和25%，表现相对较好缓凝作用。相比Al2（SO4）3和Al（NO3）3，AlCl3对净浆体积稳定性影响较为明显，导致体积膨胀与开裂。添加Al2（SO4）3和Al（NO3）3均会降低净浆早期强度，其中Al2（SO4）3弱化作用主要发生在3 h之前，而Al（NO3）3主要在12 h之前，与其较好缓凝作用相符；但二者对净浆后期强度无不利影响。添加Al（NO3）3和Al2（SO4）3能降低水化体系pH，延缓水化进程，降低水化热，并轻微抑制钾基-鸟粪石生成。铝盐中Al3+沉淀为无定型含铝物相，而NO3-和SO42-在低水灰比下分别沉淀为硝酸钾和硫酸钾，影响宏观性能。
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