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d时地聚合物的抗折强度和抗压强?分别比镍渣地聚合物提高了 32.0%?20.2%。主要是Ҏ粉煤灰颗粒表面含有的?C2S 参与反应后生更多的?胶相Q有利于改善地聚合物l构的致密性,增强与改性粉煤灰颗粒表面激发物的胶结能力。同Ӟ钙源的引 入也有助于改性粉煤灰在碱溶液的溶解,提高体系反应速率? </div> <!-- D start --> <!-- 正文 --> <div class="mainbody"> <div style="display:none"> Series No. 519 ? ? ? ? ȝ 519 ? September 2019 METAL MINE 2019 q第 9 ? Ҏ粉煤灰寚w渣基地聚合物力学性能的媄? 1 Q? 2 1Q? 2 2 3 华苏? 牧? 诸华? 梁广? 吴其? ? ? Q? 1. 江苏大学材料U学与工E学院,江苏 镇江 212013Q?. 盐城工学院材料科学与工程学院Q江?盐城224051Q? 3. 南京工业大学材料U学与工E学院,江苏 南京211816Q? ??在碱Ȁ发剂作用下制备镍渣基地聚合物Q考察自制Ҏ粉煤灰对地聚合物力学性能的媄响,q结? XRD、IR ?SEM {测试方法,对试块的微观l构和性能q行研究。结果表明:Ҏ粉煤灰的掺入有利于镍渣基地 聚合物力学性能的提高。当Ҏ粉煤灰掺量?20%时效果最佻I50 ℃养?7 d 时地聚合物的抗折强度和抗压强? 2 分别比镍渣地聚合物提高了 32.0%?20.2%。主要是Ҏ粉煤灰颗粒表面含有的?C S 参与反应后生更多的? 胶相Q有利于改善地聚合物l构的致密性,增强与改性粉煤灰颗粒表面激发物的胶结能力。同Ӟ钙源的引 入也有助于改性粉煤灰在碱溶液的溶解,提高体系反应速率? 关键?镍渣 地聚合物 Ҏ粉煤灰 中图分类?TD926.4 文献标志?A 文章~号 1001-1250Q?019Q?09-199-05 DOI 10.19614/j.cnki.jsks.201909033 Effect of Modified Fly Ash on Mechanical Properties of Nickel Slag-based Geopolymer 1 Q? 2 Zhu Huajun Liang Guangwei 1Q? 2 2 32 Zhai Munan Wu Qisheng Gao Sheng Hua Sudong Q?. School of Materials Science and EngineeringQJiangsu UniversityQZhenjiang 212013QChina;2. School of Materials Science and EngineeringQYancheng Institute of TechnologyQYancheng 224051QChina;3. School of Materials Science and EngineeringQNanjing Tech UniversityQNanjing 211816QChinaQ? Abstract The nickel slag-based geopolymer was prepared by alkali activators and the effect of self-made modified fly ashQMFAQon the mechanical properties of geopolymer was investigated. XRDQIR and SEM test techniques were adopted to study microstructure and properties of the products. The results showed that: the addition of MFA is beneficial to the mechani? cal properties improvement of nickel slag-based geopolymer. The best effect occurs with the replacement of 20% MFA. After maintaining at 50 ?for 7 daysQthe flexural strength and compressive strength of geopolymer increased by 32.0% and 20.2%Q? 2 respectively. β-C S on the surface of MFA particles took part in the reactionQwhich helped to produce more gel phase. There? foreQthe structure compactness of geopolymer was improved and the cementation ability with the MFA particle surface produc? tion were enhanced. MeanwhileQthe introduction of the calcium sources is beneficial to the dissolution of MFA in the alkali so? lution and accelerates the reaction rate of the system. Keywords Nickel slagQGeopolymerQModified fly ash 镍渣是冶炼镍铁合金过E中排放的固体废 入的研究工作Q且取得了较好的研究成果。刘梁友 Q? 1Q? Q?Q? ? 。近q来Q随着我国不锈钢业的不断发展Q镍 渣的排放量逐年增加Q仅江苏每年的排Npq? 00万t。而镍渣的传统处理方式Q填埋或露天堆放Q? {?研究发现Q镍渣作为水泥؜合材的适宜掺量? 10%Q当掺量大于 15%Ӟ强度损失率明昑֢大? Q? 3Q? 6 Yang 研究表明Q适量镍渣的掺入有利于_煤灰基? 聚合物热E_性的提高Q掺量ؓ20%时效果最佟뀂相 关研I工作的开展ؓ镍渣处理提供了新思\。但? 渣存在镁含量高、活性低{问题,D镍渣的利用率 不仅占用大量的土圎ͼq会对环境造成极大的污染, 由此带来的问题已引vC会的广泛关注? 为实现镍渣的资源化利用,研究人员开展了? 收稿日期 2019-05-07 基金目 国家自然U学基金目Q编P51502259Q,住房和城乡徏NU学技术项目(~号Q?015-K4-007Q,江苏省“六大h才高峰”项目(~号Q? 016-XCL-070Q,江苏省重点研发计划项目(~号QBE2018697Q? 作者简?牧楠(1994—)Q男Q硕士研I生。通讯作?诸华军(1981—)Q男Q副教授Q硕士研I生导师? 2 · 199 · ȝ519? ? ? ? ? 2019q第9? 偏低、应用领域偏H。部分研Ih员开展了寚w? 制备地聚合物材料的研I工作,以期提高镍渣的利 1.5Qƈ加水E释至度?8%Q陈?4 h后备用? 镍渣和粉煤灰的主要化学成分分析结果见?1Q? 镍渣及粉煤灰Ҏ前后的XRD图谱见图1Q粉煤灰? 性前后的SEM囄及改性后颗粒表面的EDS能谱? 见图2? Q?Q? 用率。王佳佳 制备的矿׃下填充用镍渣激? 胶凝材料Q其 20 ℃养?28 d 的抗压强度ؓ 3.4 MPaQ? Q? 5Q? Komnitsas 利用镍渣制备了地聚合物,?20 ℃养? Q?Q? 28 d的抗压强度达?15.9 MPaQ王?利用镍渣和碱 Ȁ发剂制备的砂材料,?20 ℃养?90 d 的抗压强 度ؓ11.3 MPa。上q研I表明,镍渣应用于地聚合? 的制备具有可行性,但存在力学强度低的缺P制约 了该材料的推q应用,相关研究工作仍需加强? 本研I用自制Ҏ粉煤灰Ҏ镍渣基地聚合? 的性能q行优化Qƈ借助 XRD、SEM ?IR {测试方 法,研究Ҏ粉煤灰寚w渣地聚合物的Ҏ作用,q? 而ؓ镍渣基地聚合物的应用提供基础数据? 1 . 1 试验原料 镍渣取自江苏宿迁华益混凝土有限公司,l行 ?? 1 星球机_磨制得镍渣微粉Q^均粒径ؓ37.45 μm? _煤Cؓ江苏南通某Ⅲ_煤灎ͼq__径? 57.07 μmQCaO含量?.57%Q属于低钙粉煤灰Q改性粉 煤灰Q由_煤灰、二水石膏及矿化剂؜合煅烧后制得? 性激发剂为市售水ȝ溶液Q初始模Cؓ 3 3.29Q密?1.69 g/cm Q试验时?NaOH 模数调节至 由图1可看出,镍渣的主要组成矿物ؓ钙镁榄 体Q试验配方见?2Q。将制备好的料注入 20 mm×20 mm×80 mm?0 mm×30 mm×30 mm的试 模中Q标准养?24 h 拆模后的试块|于 50 ℃的恒温 水ʎ׃L至不同龄期,按照水惔胶砂强度? ҎQGB/T17671-1999Q测试地聚合物的力学性能? ?X-线衍射仪(DX-2000 ?Cu 靶辐)试块样 品的物相Q用傅立叶红外光׃AQNicolet 670Q对样品 分子l构和化学键q行分析Q用扫描电子昑־? 矟뀁钙铝榴矟뀁镁铝榴石以及普通辉石等Q其中钙? 榄石矿物相较多。粉煤灰的主要组成矿物是莫来 矟뀁石英及无定形的ȝ体,Ҏ粉煤灰除含有莫? 2 4 矛_矌外,q出Cβ-C S、CaSO {物质? 由图2可看出,_煤灰颗_表面较光滑Q而改性粉 煤灰颗粒表面较粗p,p多微晶堆U构成。改性粉 煤灰颗粒表面的EDS能谱图显C其表面不仅含有Al 和Si元素Q还含有大量Ca元素。结合XRDl果分析Q?QQuanta 200Q对试块表面形貌q行观察? Ҏ粉煤灰表面的微晶主要是β-C . 2 试验Ҏ 镍渣和_煤?Ҏ粉煤灰按一定质量比? 合,在体pL量比?0.42 条g下制备地聚合? 2 S相? 2 试验l果与讨? 1 2. 1 地聚合物力学性能分析 不同原料配方的镍渣基地聚合物抗折强度见图 3Q抗压强度见?? · 200 · 牧楠等Q改性粉煤灰寚w渣基地聚合物力学性能的媄? 2019q第9? 作用较明显,掺量?20%时效果最佻I3 d ?7 d 抗压 强度分别辑ֈ22.9 MPa?2.7 MPaQ分别较镍渣地聚 合物增长?2.8%?0.2%? lg分析Q掺入适量的改性粉煤灰有利于镍? 基地聚合物力学性能的提高,且改性效果明显优? 未改性粉煤灰? 2 2 . 2 机理分析 . 2. 1 XRD分析 ?为养? d旉渣基地聚合物的XRD图谱? 由图 5 可见Q? U地聚合物的 XRD 图谱基本? |主要晶体相均为钙镁橄榄石。但是,试块N-FA- 1 2 和试?N-MFA-2 的图׃Q可以观察到衍射角ؓ 0?5的I散峰Q说明粉煤灰和改性粉煤灰的掺? 有利于体pd应过E的q行Q促q无定型凝胶相的 生成。此外,Ҏ粉煤灰中含有活性较高的β-C S? 物相Q反应后生成更多的凝胶相Q有利于地聚合物l? 构的优化。而?C S 反应后的产物 CaQOHQ则可以 作ؓ钙源增加地聚合物l构的无序性,降低_煤? 2 2 2 Q? 7Q? 4 的聚合程?Q加快体pd应速率。此外,CaSO 在碱 Q? 8Q? 环境条g下易溶解 有助?C—(AQ—S—H 凝胶? 的生成,促产物中凝胶相含量的增加。所以,Ҏ? _煤灰的掺入对地聚合物力学性能的改善效果优? 未改性粉煤灰? 由图 3 可见Q随着L龄期的g长,地聚合物? 抗折强度逐渐提高。养护龄期ؓ 3? d 的镍渣地? 合物的抗折强度均较低Q分别ؓ 5.8 MPa ?7.5 MPaQ? _煤灰的掺入Q对地聚合物抗折强度的媄响不明显Q? Ҏ粉煤灰的掺入则可有效提升镍渣基地聚合物? 抗折强度Q掺量ؓ20%时抗折强度最高,L3 d? d时分别ؓ 7.3 MPa ?.9 MPaQ较镍渣地聚合物分别 提高?5.7%?2.0%? 2 . 2. 2 IR分析 ?为养? d旉渣基地聚合物的IR图谱? - 1 由图 6 可见Q? 300? 500 cm 处的—OH、H? - 1 OH的׾~振动峰? 640 cm 处的H—OH的弯曲振 - 1 动峰׃物中的结合水造成Q? 400 cm 处的O—C? O 的׾~振动峰由样品在L或制h的部分碳? 所引v。镍渣基地聚合物的最强和ơ强特征峰出? 由图4可见Q掺10%_煤灰的试g3 d? d的抗 压强度分别比未掺_煤灰的地聚合物提高?5.9%? - 1 -1 ?984 cm ?890 cm 左右Q对?Si—O—T 键的非对 14.7%Q但随着掺量的l增大,试g的抗压强度? Q? 9Q? UC׾~振?QT表示Si或AlQ,试块N-MFA-2的Si? O—T振动峰最强,主要来源于硬化浆体中的NQCQ? 渐降低,且均低于同龄期镍渣地聚合物试件的抗压 强度Q改性粉煤灰的掺入对地聚合物抗压强度增长 · 201 · ȝ519? ? ? ? ? 2019q第9? A—S—H。此外,随着_煤灰和Ҏ粉煤灰的掺入, 地聚合物中Si—O—T键的振动C逐渐向高波数? 向偏U,且以试块 N-MFA-2 的偏Ud度最大,说明 Q? 10-11Q? 该地聚合物的反应E度较高 。可见,Ҏ粉煤灰 的掺入有助于增加镍渣基地聚合物中凝胶相,提高 试块的反应程度,从而改善其力学性能? 2 . 2. 3 SEM分析 ?为养? d旉渣基地聚合物的SEM照片? 由图 7 可见Q试?N-FA-0 的结构较qxQ分? 有少量Q状物;试块 N-FA-1 和试?N-MFA-2 ? l构则较为粗p,有大量的i状凝胶产物生成。另 一斚wQ试?N-FA-1 中粉煤灰颗粒表面被轻微R Li HaoQYang DingyiQShen WuQet al. Effect of nickel slag to wear resistance of concreteQJQ?Bulletin of the Chinese Ceramic SocietyQ? 蚀Q说明粉煤灰参与了体pd应但反应速率~慢Q仅 生成量激发物,因此对地聚合物性能的改? 效果不佳Q试块N-MFA-2中改性粉煤灰颗粒表面? 蚀则较Z重,在颗_表面Ş成了大量的碱Ȁ发 物,有利于优化改性粉煤灰颗粒与地聚合物间的胶 2 015Q?1Q?3122-3128. Q? 2Q?刘梁友,?云,?P{?镍铁渣用作؜合材Ҏ泥性能? 响的研究QJQ? 酸盐通报Q?016Q?Q?1705-1710. Liu LiangyouQLiu YunQZhang KangQet al. Influence of nickel- iron slag used as admixture on cement propertiesQJQ? Bulletin of the Chinese Ceramic SocietyQ?016Q?Q?1705-1710. Q? 12Q? l能?Q这可能是?C 2 2 S水化反应后的 CaQOHQ加 快改性粉煤灰的溶解,从而提高了体系的反应速率? Q? 3Q?Yang TQWu Q SQZhu H JQet al. Geopolymer with improved ther? mal stability by incorporating high-magnesium nickel slagQJQ?Con? struction & Building MaterialsQ?017Q?55:475-484. 3 l?? Q?Q改性粉煤灰的掺入可有效提高镍渣基地? Q? 4Q?王佳佻I刘广宇,?文,{?Ȁ发剂寚w川水淬二ơ镍渣胶l? 合物的力学性能Q且增强效果明显优于未改性粉? 灰。当Ҏ粉煤灰掺量?20%Ӟ地聚合物试块 7 d 的抗折强度和抗压强度分别?9.9 MPa ?32.7 MPaQ? 较镍渣地聚合物试块分别增长了32.0%?0.2%? 料强度的影响QJQ? 金属矿山Q?013Q?Q?159-163. Wang JiajiaQLiu GuangyuQNi WenQet al. Analysis of the influenc? es of activator on performances of Jinchuan Water-granulated sec? ondary Ni slag cemented backfilling materialsQJQ? Metal MineQ? 2 013Q?Q?159-163. 5Q?Komnitsas KQZaharaki DQPerdikatsis V. Geopolymerisation of low calcium ferronickel slagsQJQ? Journal of Materials ScienceQ? 007Q?2:3073-3082. 6Q? ?强,?峻,王登? 激发电炉镍渣的反应产物性能 JQ? 清华大学学报Q自然科学版Q?018Q?Q?593-597. Q? 2Q改性粉煤灰的掺入有利于激发反应的q? 行。掺Ҏ粉煤灰后,镍渣基地聚合物的力学性能? 到提升,β-C S、CaSO 在地聚合物中反应有利于改? Q? 2 4 2 _煤灰在性溶液中的溶解,且可以生成更多的凝胶 相。凝胶物与Ҏ粉煤灰颗粒表面的碱Ȁ发? 交叉生长Q增强物料颗_与地聚合物间的胶结能力? Q? Q? Wang QiangQYang JunQWang Dengquan. Properties of the reac? tion products of alkali- activated electric furnace nickel slagQJQ? Journal of Tsinghua UniversityQScience and technologyQ?018Q?Q? ???? 5 93-597. Q?Q? ? ,杨鼎宜,?武,{? 掺镍渣对混凝土耐磨性能的媄? Q?Q?施惠生,?明,郭晓? _煤灰基地聚合物反应机理及各l? 分作用的研究q展QJQ?酸盐学报,2013Q?Q?972-980. 研究QJQ? 酸盐通报Q?015Q?1Q?3122-3128. · 202 · 牧楠等Q改性粉煤灰寚w渣基地聚合物力学性能的媄? 2019q第9? Shi HuishengQXia MingQGuo Xiaolu. Research development on mechanism of fly ash-based geopolymer and effect of each compo? Portland cementQJQ? Journal of the European Ceramic SocietyQ? 2006Q?6:3789-3797. nentQJQ? Journal of the Chinese Ceramic SocietyQ?013Q?Q?972- 80. 8Q?Chindaprasirt PQThaiwitcharoen SQKaewpirom SQet al. Control? Q?1Q??泽,?瑜,孔凡龙,{? 激发矿渣基地质聚合物微观结 构与性能研究QJQ? 酸盐通报Q?017Q?Q? 1830-1834. 9 Q? Liu ZeQZhou YuQKong FanlongQet al. Microstructure and proper? ties of alkali-activated blast furnace slag based geopolymerQJQ? Bul? letin of the Chinese Ceramic SocietyQ?017Q?Q?1830-1834. Q?2Q?朱洪波,吴凯凡,?晨,{? 化床气相沉U法U米修饰_煤 灰及其早期水化特征EJQ? 建筑材料学报Q?016Q?Q?229-236. Zhu HongboQWu KaifanQLi ChenQet al. Nano coating fly ash by fluidized bed reactor vapor depositionQFBR-VDQand its hydration characteristics at early ageQJQ? Journal of Building MaterialsQ?016 Q?Q?229-236. ling ettringite formation in FBC fly ash geopolymer concreteQJQ? Ce? ment & Concrete CompositesQ?013Q?1:24-28. Q? 9Q?Zhang Z HQZhu Y CQYang TQet al. 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