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Article(id=1241321985750397299, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.02.022, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1695916800000, receivedDateStr=2023-09-29, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773883824050, onlineDateStr=2026-03-19, pubDate=1711900800000, pubDateStr=2024-04-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773883824050, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773883824050, creator=13701087609, updateTime=1773883824050, updator=13701087609, issue=Issue{id=1241321979433767757, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='2', pageStart='1', pageEnd='191', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773883822544, creator=13701087609, updateTime=1773884556149, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241325056454881881, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241325056454881882, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=88, endPage=91, ext={EN=ArticleExt(id=1241321986010444165, articleId=1241321985750397299, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Enhanced Extraction of Indium from Zinc Indium Ferrite by Applying a Combination of Ultrasound and Microwave, columnId=1236276106727321817, journalTitle=Mining and Metallurgical Engineering, columnName=METALLURGY, runingTitle=null, highlight=null, articleAbstract=

Alkali leaching of indium from zinc indium ferrite (ZnFe2-xInxO4) was strengthened by applying a combination of ultrasound and microwave. The results show that there are not a great amount of solid solution of indium in the octahedral lattice of ZnFe2-xInxO4, and the maximum solid solution approaches 4.0% in a mass fraction (x=0.088). The leaching rate of indium can be enhanced by the external fields in the following descending order: a combined application of ultrasound and microwave, single application of microwave, application of ultrasound followed by microwave or microwave followed by ultrasound, and single application of ultrasound. It is shown that the leaching rate of indium can be up to 56.6% with a combined application of ultrasound and microwave, but only reach 30.2% by singly applying ultrasound. During the alkaline leaching under the external fields, In3+ can be released from the lattice, while the octahedral lattice of zinc ferrite will not collapse. With a combined application of ultrasound and microwave, more In3+ can be released, leading to lattice constant becoming much smaller. The XRD spectrum shows obvious reduced intensity and rightward movement of diffraction peaks.

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在超声-微波场作用下，对铟铁酸锌（ZnFe2-xInxO4）中铟进行强化碱浸。结果表明，铟不能在ZnFe2-xInxO4八面体晶格中大量固溶，最大固溶量约4.0%（质量分数，对应x=0.088）；外场对铟浸出的促进作用大小顺序为：叠加超声-微波复合场>微波单场>顺序复合场>超声单场；在叠加超声-微波复合场下铟浸出率达56.6%，而超声单场下铟浸出率为30.2%；外场作用下碱浸，将In3+从晶格中释放出来，不会使铁酸锌的八面体晶格坍塌；叠加超声-微波复合场下浸出的In3+较多，样品的晶格常数下降较大，衍射峰强度降低与右移现象明显。

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申星梅（1982—），女，山西运城人，博士，副教授，主要研究方向为固废资源利用。E-mail：

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申星梅（1982—），女，山西运城人，博士，副教授，主要研究方向为固废资源利用。E-mail：

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申星梅（1982—），女，山西运城人，博士，副教授，主要研究方向为固废资源利用。E-mail：

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（a）超声场；（b）微波场；（c）超声-微波复合场

, figureFileSmall=f5uFEs04kFYQqTAdNG8yRw==, figureFileBig=4OpTdulxoB5+F/9kgnkvKw==, tableContent=null), ArticleFig(id=1241327503646708043, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241321985750397299, language=EN, label=null, caption=null, figureFileSmall=It5G+FM3Gx0QzlyOV8mGVA==, figureFileBig=wih8TUqALYnyBoEgieBvZg==, tableContent=null), ArticleFig(id=1241327505165046099, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241321985750397299, language=CN, label=图4, caption=不同外场浸出前后样品的XRD图谱

（a）浸出前及单场浸出后；（b）复合场浸出后

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（a）浸出前；（b）超声浸出后；（c）微波浸出后；（d）叠加复合场浸出后；（e）先超声后微波浸出后；（f）先微波后超声浸出后

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超声-微波复合场下从铟铁酸锌中强化提铟
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申星梅 1 , 彭倩柔 1 , 李乐 1 , 朱宗建 1 , 曹发斌 2 , 武杏荣 2
矿冶工程杂志 | 冶金 2024,44(2): 88-91
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矿冶工程杂志 | 冶金 2024, 44(2): 88-91
超声-微波复合场下从铟铁酸锌中强化提铟
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申星梅1 , 彭倩柔1, 李乐1, 朱宗建1, 曹发斌2, 武杏荣2
作者信息
  • 1.安徽工业大学　教育部冶金减排与资源综合利用重点实验室，安徽　马鞍山　243002
  • 2.安徽工业大学　冶金工程与资源综合利用安徽省重点实验室，安徽　马鞍山　243002

    • 申星梅（1982—），女，山西运城人，博士，副教授，主要研究方向为固废资源利用。E-mail：

Enhanced Extraction of Indium from Zinc Indium Ferrite by Applying a Combination of Ultrasound and Microwave
Xingmei SHEN1 , Qianrou PENG1, Le LI1, Zongjian ZHU1, Fabin CAO2, Xingrong WU2
Affiliations
  • 1.Key Laboratory of Metallurgical Emission Reduction & Resources Recycling of Ministry of Education, Anhui University of Technology, Ma'anshan 243002, Anhui, China
  • 2.AnHui Provincial Key Laboratory of Metallurgical Engineering & Resources Recycling, Anhui University of Technology, Ma'anshan 243002, Anhui, China
出版时间: 2024-04-01 doi: 10.3969/j.issn.0253-6099.2024.02.022
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摘要
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在超声-微波场作用下，对铟铁酸锌（ZnFe2-xInxO4）中铟进行强化碱浸。结果表明，铟不能在ZnFe2-xInxO4八面体晶格中大量固溶，最大固溶量约4.0%（质量分数，对应x=0.088）；外场对铟浸出的促进作用大小顺序为：叠加超声-微波复合场>微波单场>顺序复合场>超声单场；在叠加超声-微波复合场下铟浸出率达56.6%，而超声单场下铟浸出率为30.2%；外场作用下碱浸，将In3+从晶格中释放出来，不会使铁酸锌的八面体晶格坍塌；叠加超声-微波复合场下浸出的In3+较多，样品的晶格常数下降较大，衍射峰强度降低与右移现象明显。

铟铁酸锌  /  铟  /  复合场  /  超声  /  微波  /  碱浸

Alkali leaching of indium from zinc indium ferrite (ZnFe2-xInxO4) was strengthened by applying a combination of ultrasound and microwave. The results show that there are not a great amount of solid solution of indium in the octahedral lattice of ZnFe2-xInxO4, and the maximum solid solution approaches 4.0% in a mass fraction (x=0.088). The leaching rate of indium can be enhanced by the external fields in the following descending order: a combined application of ultrasound and microwave, single application of microwave, application of ultrasound followed by microwave or microwave followed by ultrasound, and single application of ultrasound. It is shown that the leaching rate of indium can be up to 56.6% with a combined application of ultrasound and microwave, but only reach 30.2% by singly applying ultrasound. During the alkaline leaching under the external fields, In3+ can be released from the lattice, while the octahedral lattice of zinc ferrite will not collapse. With a combined application of ultrasound and microwave, more In3+ can be released, leading to lattice constant becoming much smaller. The XRD spectrum shows obvious reduced intensity and rightward movement of diffraction peaks.

zinc indium ferrite  /  indium  /  a combined field  /  ultrasound  /  microwave  /  alkaline leaching
申星梅, 彭倩柔, 李乐, 朱宗建, 曹发斌, 武杏荣. 超声-微波复合场下从铟铁酸锌中强化提铟. 矿冶工程杂志, 2024 , 44 (2) : 88 -91 . DOI: 10.3969/j.issn.0253-6099.2024.02.022
Xingmei SHEN, Qianrou PENG, Le LI, Zongjian ZHU, Fabin CAO, Xingrong WU. Enhanced Extraction of Indium from Zinc Indium Ferrite by Applying a Combination of Ultrasound and Microwave[J]. Mining and Metallurgical Engineering, 2024 , 44 (2) : 88 -91 . DOI: 10.3969/j.issn.0253-6099.2024.02.022
正文
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铟作为世界上最稀缺的金属之一，广泛应用于武器制造、航空航天、信息产业等高科技领域，成为国家战略储备及控制出口的对象。由于没有单独矿床，铟主要从有色金属冶炼浸出渣中提取[1-2]。其中，锌冶炼浸出渣中铟以固溶形式存在于铁酸锌晶格中，形成铟铁酸锌（ZnFe2-xInxO4）[3-4]。目前，工业上采用酸浸方式提铟，存在杂质组分多且分离困难、工艺流程长等问题[5-6]。鉴于铟的两性性质，碱浸方式可有效减少铟的伴随组分，但铟铁酸锌晶格结构稳定，常规碱浸很难有效提取铟[7]，外场强化是一种有效手段。
外场强化技术能有效克服湿法过程中浸出率低、时间长等缺点，引起了国内外研究者的极大重视[8-15]。目前关于复合外场强化铟的碱性浸出研究鲜有报道。本文采用超声-微波复合场对铟铁酸锌中铟的碱浸提取进行研究，以期为铟提取技术的开发及相关理论提供科学支撑。
1　实验部分
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1.1　原料和设备
实验原料包括氧化铁、氧化铟、氧化锌和氢氧化钠，均为分析纯，购自国药集团化学试剂公司。
实验设备包括KSL-1100型马弗炉、XH-300A型电脑超声微波组合合成仪、TG16G型离心机、DHG-9030A型电热鼓风干燥箱、Ultima Ⅳ型X射线衍射仪、ARL Advant'X Intellipower 3600型X射线荧光光谱仪和MIRA3型场发射扫描电镜。
1.2　实验方法
称取一定质量的氧化锌、氧化铁和氧化铟，充分研磨混合后，放入马弗炉中900 ℃煅烧2 h，得到铟铁酸锌。将铟铁酸锌放入三口烧瓶中，加入11 mol/L氢氧化钠溶液，置于超声微波组合仪中，分别在40 ℃、不同外场下反应。结束后，以3 000 r/min转速离心分离，去离子水洗涤滤渣3次后，置于烘箱干燥。
采用X射线衍射仪检测烘干后滤渣的物相结构，采用场发射扫描电镜观察其显微形貌。采用X射线荧光光谱仪分析滤渣的化学成分，并计算铟浸出率：
式中E为铟浸出率，%；ω为滤渣中铟的质量分数，%；ω0为铟铁酸锌（ZnFe2-xInxO4）中铟的质量分数，%。
2　结果与讨论
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2.1　铟的外场碱浸原理
从铟铁酸锌中碱浸提取铟，主要分为两步：
第一步，铟的固溶释放。一般而言，铟铁酸锌的八面体晶格结构非常稳定，常规碱浸很难将固溶于晶格中的铟释放出来。本实验加入外场强化手段促进铟的释放，生成In（OH）3：
第二步，In（OH）3的溶解。In（OH）3在NaOH中的溶解度[16]如图1所示。
In（OH）3具有两性化合物的性质，在低浓度碱液中不溶，在高浓度碱液中溶解进入液相生成铟酸盐，与固相浸出渣分离：
此外，如果碱液浓度过高，In（OH）3又转变为微溶的铟盐Na3In（OH）6·2H2O：
2.2　铟的固溶量分析
图2为不同固溶量（x=0.05，0.088，0.1，0.2，0.3）下铟铁酸锌（ZnFe2-xInxO4）样品的XRD图谱。从图2可以看出，铟固溶量较低（x=0.05，0.088）时，样品为铟铁酸锌单相，没有杂峰出现；在铁酸锌晶格中，铟一般以间隙固溶或置换固溶的形式存在[17]。铟固溶量增至x=0.1后，样品在2θ=21°左右出现新的漫散射峰，推测铟在铁酸锌晶格中的固溶量已达到饱和，且已有少量铟游离于铁酸锌晶格之外，少量游离铟所形成的排列长程无序，因此出现漫散射峰。x=0.2时，除了2θ=21°处的漫散射峰外，分别在2θ=31°，35°，51°，61°处出现了In2O3的特征峰，表明此时铟已无法固溶于铁酸锌晶格中；x=0.3时，2θ=21°的漫散射峰已变为较尖锐的衍射峰，此时样品中ZnFe2-xInxO4和In2O3两相并存。
由上可知，铟不能在ZnFe2-xInxO4八面体晶格中大量固溶，其固溶量极低，x=0.088是铟在铁酸锌晶格中的最大固溶量。基于此，本文选择x=0.088进行后续实验，换算为铟的质量分数为4.0%。
2.3　外场作用下铟的碱性浸出率
图3为不同外场下铟浸出率随浸出时间的变化曲线。不加外场时，铟的碱性浸出率较低，10 min时仅2.6%，150 min时为20.5%。加入600 W超声场后，浸出率略有提高，但增加幅度不大。超声功率提高至1 000 W时，30 min浸出率有明显提升，达30.2%，但随后浸出率呈逐渐下降趋势，150 min时降至21.7%；推测原因是，反应生成的铟酸盐NaInO2在持续超声作用下不稳定，又再次转化为In（OH）3沉淀。1 400 W超声场中铟浸出率在10 min、20 min时略高，随后均低于1 000 W超声场的浸出率，这可能也与NaInO2的转化有关。100 W微波场中浸出10 min时，铟浸出率提升至35.0%，比无外场作用下的浸出率明显提高；随着微波浸出时间延长，浸出率逐渐提高，90 min时达52.1%；继续延长浸出时间，浸出率无明显变化。提高微波功率至300 W、500 W，相对100 W微波场，浸出率变化不大。超声-微波复合场下浸出铟，选择单场下的适宜条件：超声功率1 000 W、微波功率100 W，采用了3种复合方式：叠加复合、先超声后微波、先微波后超声，可以看出，叠加复合方式下的浸出率最高，150 min时达56.6%，表现出一定的叠加效应。超声波属于机械波，其空化作用可使铟铁酸锌晶格的局部瞬间产生高温高压，该能量与晶格振动发生能量交换时，含铟晶格键易被破坏；微波属于电磁波，其能量可使铟铁酸锌晶格发生高速振动，从而将微波能转化为热能，铟铁酸锌中不同组元对微波的选择性吸收造成了晶格局部能量和温度的不均衡，易产生结构缺陷。因此，超声和微波的叠加效应为铟向溶液中的迁移打开了通道。在先超声后微波、先微波后超声这两种复合方式下，浸出率较单场没有优势，其中先超声后微波时最高浸出率47.0%，而先微波后超声时最高浸出率仅32.6%。由此可见，叠加复合场对铟碱性浸出的强化作用更强，而顺序复合场的强化作用较弱。超声、微波单场均能促进铟的碱性浸出反应，微波场的效果更明显，促进作用大小顺序为：叠加复合场>微波单场>顺序复合场>超声单场。
2.4　外场作用下碱浸渣的表征
图4为不同外场浸出前后样品的XRD图谱。从图4可以看出，外场强化浸出后，浸出渣的特征峰均与浸出前的特征峰一致，表明外场碱浸虽然将部分In3+从晶格中释放出来，但并不会使铁酸锌的八面体晶格坍塌。
外场强化浸出后样品的衍射峰均出现了轻微右移，表明样品的晶格常数有所下降。这是因为In3+半径（0.082 nm）略大于Fe3+半径（0.067 nm），当较大的In3+从晶格中释放出来后，样品的晶格常数减小。根据布拉格公式2dsinθ=nλ，d减小，则θ增大，衍射峰发生右移。其中叠加复合场样品的衍射峰右移更明显，这与其浸出率结果相符。同时，外场浸出后样品的衍射峰强度有所降低，表明样品的晶格结构出现缺陷，这是由部分In3+从晶格中释放所致。
图5为不同外场浸出前后样品的SEM图片。浸出前样品为不规则球形颗粒，粒径0.5～1 μm，偶见尺寸大于2 μm的颗粒，颗粒间较为分散，且颗粒的轮廓与边界较为清晰。超声单场碱浸后，样品颗粒紧密聚集在一起，大部分颗粒的轮廓与边界较为模糊。微波单场及不同方式复合场碱浸后，颗粒间也出现聚集现象，但颗粒轮廓与边界尚清晰。微波单场碱浸与先超声后微波浸出所得样品中出现针棒状物，推测其为残留的氢氧化钠。
3　结论
收起
1）铟不能在ZnFe2-xInxO4八面体晶格中大量固溶，最大固溶量约为4.0%（质量分数，对应x=0.088）。
2）外场对铟碱性浸出反应的促进作用大小顺序为：叠加复合场>微波单场>顺序复合场>超声单场。叠加复合场下铟浸出率为56.6%，超声单场下铟浸出率为30.2%。
3）外场作用下碱浸，将In3+从ZnFe2-xInxO4晶格中释放出来，但并不会使铁酸锌的八面体晶格坍塌。由于叠加复合场下浸出的In3+更多，其衍射峰强度降低与右移现象明显。
基金
收起
  • 国家自然科学基金(51302003)
  • 安徽省高校优秀青年人才项目(gxyqZD2020017)
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doi: 10.3969/j.issn.0253-6099.2024.02.022
  • 接收时间：2023-09-29
  • 首发时间：2026-03-19
  • 出版时间：2024-04-01
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  • 收稿日期：2023-09-29
基金
国家自然科学基金(51302003)
安徽省高校优秀青年人才项目(gxyqZD2020017)
作者信息
    1.安徽工业大学　教育部冶金减排与资源综合利用重点实验室，安徽　马鞍山　243002
    2.安徽工业大学　冶金工程与资源综合利用安徽省重点实验室，安徽　马鞍山　243002
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2种不同金属材料的力学参数
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species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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