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Article(id=1321935466828513618, tenantId=1146029695717560320, journalId=1220038251117760515, issueId=1321927083589227197, articleNumber=null, orderNo=null, doi=10.11868/j.issn.1001-4381.2024.000342, pmid=null, cstr=32421.14.j.issn.1001-4381.2024.000342, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1715529600000, receivedDateStr=2024-05-13, revisedDate=null, revisedDateStr=null, acceptedDate=1719763200000, acceptedDateStr=2024-07-01, onlineDate=1793103575664, onlineDateStr=2026-10-27, pubDate=1776614400000, pubDateStr=2026-04-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793103575664, onlineIssueDateStr=2026-10-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793103575664, creator=13701087609, updateTime=1793103575664, updator=13701087609, issue=Issue{id=1321927083589227197, tenantId=1146029695717560320, journalId=1220038251117760515, year='2026', volume='54', issue='4', pageStart='1', pageEnd='345', issueExtLink='null', onlineDate='null', pubDate='1776614400000', pubDateStr='2026-04-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793101576945, creator='13701087609', updateTime=1793101576945, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=338, endPage=345, ext={EN=ArticleExt(id=1321935467025645907, articleId=1321935466828513618, tenantId=1146029695717560320, journalId=1220038251117760515, language=EN, title=Preparation of cadmium and sulfur deficient CdS for photocatalytic reduction of CO2, columnId=1220689384450478826, journalTitle=Journal of Materials Engineering, columnName=RESEARCH ARTICLE, runingTitle=null, highlight=null, articleAbstract=

Converting CO₂ into C1 chemicals such as CO，CH₄，and CH₃OH using solar energy as the driving force is an effective strategy to alleviate the greenhouse effect and energy shortage crisis. However，single-component catalysts face challenges in photocatalytic CO2 reduction including limited light absorption capacity，easy recombination of photogenerated carriers，and low overall catalytic efficiency. Constructing high-efficiency catalysts to improve photocatalytic CO₂ reduction performance is therefore crucial. In this study，CdS-0.25 with sulfur vacancies and CdS-2 with cadmium vacancies are successfully synthesized via a hydrothermal method by adjusting the ratio of cadmium and sulfur precursors. Characterization analysis shows that compared with CdS-2 with cadmium vacancies，CdS-0.25 with sulfur vacancies exhibits stronger solar light absorption capacity and effectively suppresses the recombination of photogenerated electrons and holes. First-principles calculations demonstrate that sulfur vacancies have better adsorption capacity for CO₂ reactant molecules. The production rates of CO，CH₄，and H₂ from CO₂ reduction over CdS-0.25 are 1.69，0.41，0.11 µmol/（g·h），respectively. These values are 15.8，2，and 1.2 times higher than those of CdS-2. This work provides insights for the design of high-efficiency defective materials for photocatalytic CO₂ reduction.

, authors=Lan GUO1, 2, Linyu WEI1, authorsList=Lan GUO, Linyu WEI, authorCompany=null, correspAuthors=Lan GUO, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1321935470829879658, articleId=1321935466828513618, tenantId=1146029695717560320, journalId=1220038251117760515, language=CN, title=镉硫缺陷CdS的制备及光催化还原CO2性能, columnId=1220689384622445292, journalTitle=材料工程, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

以太阳光为驱动力将CO2转化为CO、CH4、CH3OH等C1化学品是当前缓解温室效应及能源短缺危机的有效策略。而单一催化剂在光还原CO2过程中存在对光吸收能力有限、光生载流子易复合及整体催化效率低等问题，因此构建高效催化剂提高光还原CO2性能是关键。本研究通过调控镉硫前驱体比例，采用水热法成功合成具有硫空位的CdS-0.25和具有镉空位的CdS-2。通过表征分析发现，在该体系中相较镉空位CdS-2，硫空位CdS-0.25对太阳光具有更强吸收能力，同时能够有效抑制其光生电子-空穴的复合；第一性原理计算表明S空位更能良好吸附反应物气体分子CO2。CdS-0.25中CO2还原产物CO、CH4、H2的生成速率分别为1.69、0.41、0.11 µmol/（g·h），比CdS-2产物分别提升了15.8、2、1.2倍。该工作为设计高效缺陷材料提供了思路。

, authors=郭兰1, 2, 魏琳钰1, authorsList=郭兰, 魏琳钰, authorCompany=null, correspAuthors=郭兰, authorNote=null, correspAuthorsNote=
郭兰（1993—），女，助教，硕士，研究方向为能源催化材料的制备与应用，联系地址：四川省宜宾市三江新区大学路5号宜宾学院二期（644000），E-mail：
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Interfaces，2017，9（33）：27773-27783., articleTitle=Fabrication of heterogeneous-phase solid-solution promoting band structure and charge separation for enhancing photocatalytic CO2 reduction：a case of Zn X Ca1- X In2S4, refAbstract=null), Reference(id=1321935482116751814, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, doi=null, pmid=null, pmcid=null, year=2017, volume=349, issue=null, pageStart=208, pageEnd=217, url=null, language=null, rfNumber=[36], rfOrder=41, authorNames=CAO S W, LI Y, ZHU B C, journalName=Journal of Catalysis, refType=null, unstructuredReference=CAO S W， LI Y， ZHU B C，et al.Facet effect of Pd cocatalyst on photocatalytic CO2 reduction over g-C3N4 ［J］.Journal of Catalysis，2017，349：208-217., articleTitle=Facet effect of Pd cocatalyst on photocatalytic CO2 reduction over g-C3N4, refAbstract=null), Reference(id=1321935482209026503, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, doi=null, pmid=null, pmcid=null, year=2020, volume=65, issue=6, pageStart=522, pageEnd=532, url=null, language=null, rfNumber=[37], rfOrder=42, authorNames=郭兰, 曹玥晗, 淡猛, journalName=科学通报, refType=null, unstructuredReference=郭兰，曹玥晗，淡猛，等.Co/CdS中Co-S键促进载流子分离增强光还原CO2性能［J］.科学通报，2020，65（6）：522-532., articleTitle=Co/CdS中Co-S键促进载流子分离增强光还原CO2性能, refAbstract=null), Reference(id=1321935482288718280, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, doi=null, pmid=null, pmcid=null, year=2020, volume=65, issue=6, pageStart=522, pageEnd=532, url=null, language=null, rfNumber=[37], rfOrder=43, authorNames=GUO L, CAO Y H, DAN M, journalName=Chinese Science Bulletin, refType=null, unstructuredReference=GUO L， CAO Y H， DAN M，et al.Promoting charge carriers transfer of Co-S bonds in Co/CdS for enhanced photocatalytic CO2 reduction［J］.Chinese Science Bulletin，2020，65（6）：522-532., articleTitle=null, refAbstract=null)], funds=[Fund(id=1321935476534133148, 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articleId=1321935466828513618, language=EN, label=Fig.1, caption=XRD patterns of CdS with different proportions, figureFileSmall=va+HD+gBJKoS/dC4nti5tw==, figureFileBig=UD6MiJteU9JB6HXYs7d9DA==, tableContent=null), ArticleFig(id=1321935472662790533, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, language=CN, label=图1, caption=不同比例硫化镉的XRD图谱, figureFileSmall=va+HD+gBJKoS/dC4nti5tw==, figureFileBig=UD6MiJteU9JB6HXYs7d9DA==, tableContent=null), ArticleFig(id=1321935472864117126, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, language=EN, label=Fig.2, caption=SEM（1），HRTEM（2），and SAED patterns（3） of CdS with different proportions, figureFileSmall=ac7GnHjOStZkL9P+Y0Jqcg==, figureFileBig=JgX3am6TsXh9Fi9m/VqUpA==, tableContent=null), ArticleFig(id=1321935472952197511, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, language=CN, label=图2, caption=不同比例CdS的SEM（1）、HRTEM（2）、SAED（3）图（a）CdS-0.25；（b）CdS-2

（a）CdS-0.25；（b）CdS-2

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articleId=1321935466828513618, language=CN, label=图10, caption=不同摩尔比CdS样品的瞬态光电流（a）和阻抗（b）谱, figureFileSmall=TzZ0k8cclKCL+UBjOgtHPw==, figureFileBig=83KVPaQY9VUPPjxNbDxusA==, tableContent=null), ArticleFig(id=1321935476089536920, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, language=EN, label=Fig.11, caption=CO2 adsorption on different vacancy cadmium sulfide surface, figureFileSmall=2TRBfFVny/HlHVebDaTI9g==, figureFileBig=glxdxSL/4eWjfYS2yFVLUA==, tableContent=null), ArticleFig(id=1321935476156645785, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, language=CN, label=图11, caption=不同空位缺陷CdS表面CO2吸附模型（a）CdS-0.25；（b）CdS-2

（a）CdS-0.25；（b）CdS-2

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Comparison of photocatalytic reduction of CO2 with different catalysts

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PhotocatalystConditionSystemProductProduction rate/（µmol·g-1·h-1）Ref.
Pd0.6Bi1.4O2Cl1.4Visible lightCO2，H2OCO，CH3OH0.6，0.9［30］
CdS/A-GOVisible lightCO2，H2OCO2.2［31］
CdS-TiO2-NSFull spectrumCO2，H2OCH4，CO0.54，3.62［32］
Pt-Cu2O/TiO2UV-lightCO2，H2OCH4，CO1.42，0.05［33］
Co3O4/Co/TiO2Full spectrumCO2，H2OCH40.25［34］
Zn0.4Ca0.6In2S4Visible lightCO2，H2OCH4，CO0.87，0.22［35］
Pd/C3N4Visible lightCO2，H2OCH4，CH3OH0.4，3.17［36］
CdS-0.25Full spectrumCO2，H2OCO，CH41.69，0.41This work
), ArticleFig(id=1321935476399915419, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935466828513618, language=CN, label=表1, caption=

不同催化剂对CO2光催化还原效果的比较

, figureFileSmall=null, figureFileBig=null, tableContent=
PhotocatalystConditionSystemProductProduction rate/（µmol·g-1·h-1）Ref.
Pd0.6Bi1.4O2Cl1.4Visible lightCO2，H2OCO，CH3OH0.6，0.9［30］
CdS/A-GOVisible lightCO2，H2OCO2.2［31］
CdS-TiO2-NSFull spectrumCO2，H2OCH4，CO0.54，3.62［32］
Pt-Cu2O/TiO2UV-lightCO2，H2OCH4，CO1.42，0.05［33］
Co3O4/Co/TiO2Full spectrumCO2，H2OCH40.25［34］
Zn0.4Ca0.6In2S4Visible lightCO2，H2OCH4，CO0.87，0.22［35］
Pd/C3N4Visible lightCO2，H2OCH4，CH3OH0.4，3.17［36］
CdS-0.25Full spectrumCO2，H2OCO，CH41.69，0.41This work
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镉硫缺陷CdS的制备及光催化还原CO2性能
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郭兰 1, 2 , 魏琳钰 1
材料工程 | 研究论文 2026,54(4): 338-345
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材料工程 |研究论文 2026 , 54 (4) : 338 -345
镉硫缺陷CdS的制备及光催化还原CO2性能
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郭兰1, 2 , 魏琳钰1
作者信息
  • 1.宜宾学院 材料与化学工程学院，四川 宜宾 644000
  • 2.宜宾学院 国有资产与实验设备管理处，四川 宜宾 644000
通讯作者:
郭兰（1993—），女，助教，硕士，研究方向为能源催化材料的制备与应用，联系地址：四川省宜宾市三江新区大学路5号宜宾学院二期（644000），E-mail：
Preparation of cadmium and sulfur deficient CdS for photocatalytic reduction of CO2
Lan GUO1, 2 , Linyu WEI1
Affiliations
  • 1.School of Materials and Chemical Engineering，Yibin College，Yibin 644000，Sichuan，China
  • 2.State Assets and Laboratory Equipment Management Department，Yibin College，Yibin 644000，Sichuan，China
出版时间: 2026-04-20 doi: 10.11868/j.issn.1001-4381.2024.000342
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摘要
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以太阳光为驱动力将CO2转化为CO、CH4、CH3OH等C1化学品是当前缓解温室效应及能源短缺危机的有效策略。而单一催化剂在光还原CO2过程中存在对光吸收能力有限、光生载流子易复合及整体催化效率低等问题，因此构建高效催化剂提高光还原CO2性能是关键。本研究通过调控镉硫前驱体比例，采用水热法成功合成具有硫空位的CdS-0.25和具有镉空位的CdS-2。通过表征分析发现，在该体系中相较镉空位CdS-2，硫空位CdS-0.25对太阳光具有更强吸收能力，同时能够有效抑制其光生电子-空穴的复合；第一性原理计算表明S空位更能良好吸附反应物气体分子CO2。CdS-0.25中CO2还原产物CO、CH4、H2的生成速率分别为1.69、0.41、0.11 µmol/（g·h），比CdS-2产物分别提升了15.8、2、1.2倍。该工作为设计高效缺陷材料提供了思路。

镉空位  /  硫空位  /  缺陷CdS  /  光催化还原CO2

Converting CO₂ into C1 chemicals such as CO，CH₄，and CH₃OH using solar energy as the driving force is an effective strategy to alleviate the greenhouse effect and energy shortage crisis. However，single-component catalysts face challenges in photocatalytic CO2 reduction including limited light absorption capacity，easy recombination of photogenerated carriers，and low overall catalytic efficiency. Constructing high-efficiency catalysts to improve photocatalytic CO₂ reduction performance is therefore crucial. In this study，CdS-0.25 with sulfur vacancies and CdS-2 with cadmium vacancies are successfully synthesized via a hydrothermal method by adjusting the ratio of cadmium and sulfur precursors. Characterization analysis shows that compared with CdS-2 with cadmium vacancies，CdS-0.25 with sulfur vacancies exhibits stronger solar light absorption capacity and effectively suppresses the recombination of photogenerated electrons and holes. First-principles calculations demonstrate that sulfur vacancies have better adsorption capacity for CO₂ reactant molecules. The production rates of CO，CH₄，and H₂ from CO₂ reduction over CdS-0.25 are 1.69，0.41，0.11 µmol/（g·h），respectively. These values are 15.8，2，and 1.2 times higher than those of CdS-2. This work provides insights for the design of high-efficiency defective materials for photocatalytic CO₂ reduction.

cadmium vacancy  /  sulfur vacancy  /  defect CdS  /  photocatalytic reduction CO2
郭兰, 魏琳钰. 镉硫缺陷CdS的制备及光催化还原CO2性能. 材料工程, 2026 , 54 (4) : 338 -345 . DOI: 10.11868/j.issn.1001-4381.2024.000342
Lan GUO, Linyu WEI. Preparation of cadmium and sulfur deficient CdS for photocatalytic reduction of CO2[J]. Journal of Materials Engineering, 2026 , 54 (4) : 338 -345 . DOI: 10.11868/j.issn.1001-4381.2024.000342
正文
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工业化进程的高速发展，过度消耗化石燃料造成CO2大量排放引发全球温室效应加剧，触发全球能源危机等问题已经受到各国政府及研究者们的广泛关注［1-3］。为实现国家提出的碳达峰、碳中和目标，可以通过多种催化技术，如电催化、光催化、热催化、压催化及耦合等新型催化技术将CO2转换为高附加值产品。其中，利用光催化技术以源源不尽的太阳能为驱动力将CO2转化为CO、CH4、CH3OH等C1化学品被普遍认为是能同时解决能源和环境问题的一个绿色策略［4-8］。由于CO2分子具有线性结构，热稳定性极强，C═O双键的断裂需要高达750 kJ/mol的能量，因此光催化还原CO2存在催化效率低的问题［9］。解决此难题，催化剂则是关键。
在光还原CO2和光解水产氢领域，硫化镉因对太阳光响应良好（禁带宽度2.4 eV）而备受研究者青睐［9-10］。但是研究发现CdS在不进行任何改性下，在光催化过程会伴随严重的光腐蚀问题，主要是因其光生电子-空穴复合率高，进而使纯相的CdS非常不稳定，不利于光催化反应的进行［11-12］。对此，可以通过引入贵金属、过渡金属等作为助催化剂或者构建异质结/同质结等方式去改善CdS［13-16］，但是这些都存在成本高、经济效益差的问题。近年的研究发现，缺陷可以作为电荷捕获中心，抑制材料中光生电子-空穴的复合，进而促进光催化性能的提升［17-22］。然而多数工作主要集中于研究催化剂中单一空位缺陷类型对材料催化性能的影响。而对于材料中分别存在阴阳离子空位缺陷时，对材料光电性质和催化性能的影响非常具有研究价值。
基于以上考虑，本工作采用水热法调控前驱体镉和硫比例构建具有镉空位或硫空位的缺陷化CdS，研究不同空位缺陷的引入对材料光电性质的改变及催化性能的影响。测试发现，阳离子镉空位的引入相对阴离子硫空位并未表现出优异的光电化学性质，而硫空位的引入不仅可以促进CdS对光的吸收，还能促进其载流子的有效分离，抑制光生电子-空穴的复合，使得更多的电子参与反应，进而提高光催化还原CO2的性能。
1 实验材料与方法
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1.1 实验原料
五水氯化镉（CdCl2·5H2O），分析纯，购自上海阿拉丁化学试剂有限公司；九水硫化钠（Na2S·9H2O）、盐酸、N，N-二甲基甲酰胺（DMF），分析纯，均购自成都科龙化工有限公司；实验试剂直接使用，未纯化处理。
1.2 镉硫缺陷CdS的制备
首先以水为溶剂采用水热法，以前驱体CdCl2·5H2O中镉源量不变。通过控制NaS2·9H2O前驱体硫的含量制备不同镉硫摩尔比含量的缺陷CdS催化剂。以硫化镉中Cd与S的摩尔比为1∶0.5为例，首先将4 mmol的CdCl2·5H2O溶于20 mL的去离子水中，调节pH=1，标记为A液。再将2 mmol的Na2S·9H2O加入20 mL的去离子水中，标记为B液。然后将B液一滴一滴缓慢滴入A液中，匀速搅拌使混合溶液变成橙黄色的悬浮液。最后将悬浮液转移至50 mL的聚四氟乙烯高压反应釜中，放置于140 ℃的烘箱中保温18 h。待反应完成后自然冷却到室温，通过离心法回收得到固体样品。最后用乙醇和去离子水多次清洗得到固体样品，并在60 ℃真空干燥箱保温24 h得到黄色粉末，标记为CdS-0.5。以相同的方法合成CdS-0.125、CdS-0.25、CdS-1、CdS-2等样品。
1.3 材料表征方法
采用X射线衍射仪（PRO MPD型）对催化材料的晶体结构进行物相分析；采用扫描电子显微镜（ZEISS EV0 MA15型）和透射电子显微镜（G2 F30型）对材料的微观形貌、尺寸进行分析；通过电子自旋共振谱（ESR，JES FA200型）分析硫化镉缺陷类型；紫外-可见漫反射光谱（UV-vis DRS，UV-2600型）和荧光光谱仪（PL，F-7000型，360 nm室温激发）对镉硫缺陷硫化镉的光学性质进行分析；采用X射线光电子能谱（ESCALAB 250型）分析催化剂元素化学态信息（以C 1s峰284.8 eV为标准）。
1.4 光催化还原CO2性能测试实验
采用石英玻璃反应器作为反应容器，体积大约在270 mL，保持常温常压密闭状态进行光还原CO2性能评价测试。第1步将30 mg催化剂均匀铺在含有适量水的培养皿中（面积为6 cm2），于真空干燥箱中采用70 ℃进行烘干。第2步在反应器底部放置1 mL水，并将干燥好的催化剂放置在反应器底部。向反应器中通氩气将残余空气反复抽排干净。最后向反应器中通1%浓度的CO2水汽至充满整个反应器。采用300 W氙灯为光源，模拟太阳光辐照（波长320~780 nm） 600 mW/cm2，辐照窗口约为5 cm2，将反应器置于搅拌台上边搅拌边光照，每隔2 h从反应器中取1 mL气体进样。采用GC7900气相色谱（天美）配备火焰离子化检测器（FID，检测分析CO和CH4）和热导检测器（TCD，检测分析H2）对产物进行定性定量分析。同位素测试实验采用与上述反应装置相同的设备，以13CO2为碳源，产物采用质谱（OmniStarTM）进行分析。
1.5 光电化学测试实验
采用CHI660E型电化学工作站对镉硫缺陷硫化镉的电化学阻抗谱（EIS）和瞬态光电流（I-t）进行分析。实验在300 W氙灯下进行。采用以铂丝为对电极，饱和甘汞电极（SCE）为参比电极，以涂有不同缺陷CdS的ITO导电玻璃为工作电极的传统三电极系统，样本有效面积为1 cm2，电解液为1.2 mol/L的Na2SO3溶液。缺陷CdS膜的制作：首先，超声清洗ITO玻璃，以除去表面杂质。然后，称量100 mg的缺陷CdS粉末，滴加几滴DMF溶液于研钵中研磨粉末至黏稠的浆液，即完成膜液的制备。将膜液均匀涂在ITO玻璃上，用刮刀刮涂厚度为50 µm的薄膜。室温下自然干燥1 h，放入真空干燥箱中120 ℃保温3 h。
1.6 第一性原理（DFT）计算
采用Materials Studio中CASTEP模块进行计算，使用广义梯度近似（GGA）中PBE泛函对各缺陷硫化镉进行模拟。整个计算优化过程中能量收敛值是1.0×10-5 eV/atom，截断能为400 eV，k点为2×2×1，真空层厚度设置为1.5 nm，收敛精度为0.02 eV/nm。镉硫空位缺陷CdS-0.25和CdS-2的形成能（Ef）和反应物气体分子的吸附能Eads，如式（1），（2）所示：
Ef=Etot-ES/ECd
Eads=Esurf+mole-Esurf-Emole
式中：Etot为优化后完整CdS的总能量；ES和ECd分别表示单个S和单个Cd原子构型的能量；Esurf+mole为反应物CO2气体分子吸附于有空位缺陷的CdS表面的总能量；Esurf为缺陷CdS表面的能量；Emole为单个CO2气体分子的能量。
2 结果与分析
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2.1 物相结构分析
图1是制得不同隔硫比含量的硫化镉催化剂XRD图。所得硫化镉样品各个衍射峰的位置均与标准六方相（PDF# 65-3414）CdS相对应，无杂质峰出现，即样品皆为六方相硫化镉，表明镉硫比含量的改变并没有改变硫化镉的本征结构。从图中发现随着镉硫比中S含量的增加，CdS（002）晶面的衍射峰强度呈现逐渐增强的趋势，最后在CdS-2中（002）晶面峰强度最高。同时发现不同镉硫比含量CdS的各个衍射峰出现宽化现象，表明硫含量的增大会让CdS的结晶度变弱，其衍射峰的强度和结晶度也会受S含量改变的影响。
2.2 微观形貌结构分析
为了探究不同镉硫比含量硫化镉微观形貌结构的差异，结合XRD结果，并以适当镉硫比例的CdS-0.25和CdS-2催化剂做了进一步的表征分析。从SEM图中可以看出CdS-0.25和CdS-2样品都是由一个个小球堆叠而成，并随着S含量的增加，小球粒径也逐渐变大（图2（a-1），（b-1））。高倍透射电子显微镜（HRTEM）图中发现，CdS-0.25和CdS-2都有着明暗清晰的晶格条纹，但在边缘处都存在明显的晶格模糊和晶格畸变等缺陷（图2（a-2），（b-2））。选区电子衍射（SAED）图中可看出，当S的含量增加，衍射环花样变得模糊，说明催化剂在转向非晶化（图2（a-3），（b-3））。这也进一步说明前驱体镉硫比不对等的情况下，催化剂中存在缺陷。为了进一步确定缺陷的类型，采用电子自旋共振谱（ESR）做了进一步探究。
图3为CdS-0.25和CdS-2的ESR图，CdS-0.25和CdS-2的g值信号分别为2.03和2.24，其中g=2.03对应S空位的信号［23-24］，而g=2.24通常对应过渡金属阳离子的空位信号，因此在这里对应Cd2+空位信号［25-29］，说明通过调控前驱体镉硫比含量可成功制得含镉空位和硫空位缺陷的硫化镉催化剂，即材料中某一原料过量，成核过程中另一元素将形成缺陷。
通过第一性原理计算分别构建了具有硫或镉空位的硫化镉模型，探究镉硫空位在硫化镉中能否稳定存在，结果如图4所示。含硫空位的CdS-0.25形成能为-6.28 eV，镉空位CdS-2的形成能为-4.31 eV，通常能量值为负说明该结构模型可自发形成，数值越负表示其结构越稳定，表明具有硫空位的CdS-0.25稳定性更好。
2.3 元素表面化学态分析
采用XPS进一步分析了镉硫空位缺陷的引入对CdS中各元素化学态的影响。从图5（a）中看到相较CdS-1的S 2p轨道向高结合能方移动了0.29 eV，而CdS-2的S 2p轨道只移动了0.03 eV。再结合图5（b）中Cd的3d轨道精细谱发现与CdS-1相比，CdS-0.25的Cd 3d轨道向高结合能方移动了0.4 eV，而CdS-2的Cd 3d轨道略微向低结合能方向进行了移动。以上说明镉硫空位的引入使得缺陷硫化镉中Cd、S元素周围电子不断迁移至S空位处，使得Cd、S元素周围电荷密度排布发生变化，而元素电荷密度改变将使催化活性位点的电荷富集状态发生改变，最终使材料催化活性出现差异。
2.4 光催化还原CO2性能研究
通过光还原CO2性能测试实验研究不同空位缺陷硫化镉的光催化性能，如图6所示。从图6（a）~（c）中发现，在300 W氙灯全光谱光照8 h后，产物主要以CO为主，当Cd∶S摩尔比大于1时（CdS-0.125、CdS-0.25、CdS-0.5）光催化还原CO2的产物CO含量显然高于CdS-1和CdS-2；对于产物CH4和H2的产量只有CdS-0.25最为显著。光照8 h后，CdS-0.25中CO、CH4、H2的生成速率分别为1.69、0.41、0.11 µmol/（g·h），比CdS-2分别提升了15.8、2、1.2倍。该催化剂与已报道文献中材料光还原CO2性能相比，具有较好的催化性能，详见表1［30-36］。图6（d）中进一步做了CO2还原的长时间实验，探究CdS-0.25催化剂的稳定性，发现反应10 h后，催化活性增长速率开始变得缓慢，经过3次循环测试，催化剂活性能持续24 h，详见图7。
图8是保持上述测试条件，仅用13CO2代替12CO2做的同位素实验。图中质荷比（m/z）为2的信号对应H2，质荷比为17的信号对应13CH4，质荷比为29的信号对应13CO，表明产物CO、CH4中碳源均来自反应器中反应物CO2。
2.5 机理分析
影响光催化活性的两个重要因素是半导体催化剂对太阳光的吸收能力和光生电子-空穴的复合率。图9通过紫外可见漫反射光谱和光致发光光谱探究了镉硫空位缺陷CdS光学性质差异情况。图9（a）中所有催化剂都具有大于500 nm的吸收边，对太阳光具有良好响应，只有硫空位缺陷CdS-0.25具有最大吸收边，说明硫空位的引入扩大了CdS对太阳光的吸收。再结合图9（b）中光致发光光谱，发现CdS-0.25的荧光峰强度明显低于CdS-2，表明CdS-0.25中光生载流子复合率得到抑制，使得更多的电子参与反应，利于CdS-0.25光催化还原CO2反应的进行，这与光催化还原CO2性能测试实验结果相匹配。
图10通过瞬态光电流和电化学阻抗进一步探究了镉硫空位硫化镉之间存在活性差异的原因。从瞬态光电流中可以发现，经过多个循环测试，样品依然保持平稳的光电流，表明缺陷硫化镉的稳定性相对较好，与长时间实验相匹配。特别是含硫空位的CdS-0.25的光电流强度显著高于CdS-2，表明CdS-0.25材料表面光生载流子更多（图10（a））。再结合图10（b）电化学阻抗谱，在光场和暗场条件下CdS-0.25的圆弧半径最小。而通常圆弧半径的大小对应的是阻抗值的大小，圆弧半径越小，阻抗值越小，阻抗值越小，对材料中载流子的运动阻碍越小，载流子迁移速度更快［37］。上述结果表明CdS-0.25材料表面富集大量光生载流子，更多的电子可参与光还原CO2反应，即CdS-0.25光催化还原CO2的性能最佳。
影响气固相催化反应一个非常重要的因素是反应物气体分子能否在催化剂表面有效吸附。故CO2气体分子在催化剂的表面反应往往是限制CO2催化效率的关键步骤，因此构建了CO2分别在CdS-0.25和CdS-2表面的吸附构型。如图11所示，通过计算发现CO2距离CdS-0.25表面距离为0.194 nm，吸附能为-0.12 eV，距离CdS-2表面的距离为0.287 nm，吸附能为-0.05 eV。吸附能值越负表明材料对CO2的吸附作用力越强，说明S空位的引入，提高了催化剂对CO2的吸附能力，进而有利于后续反应的进行。
3 结论
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（1）本研究通过调控前驱体镉和硫的含量比，制备出具有硫空位的CdS-0.25和具有镉空位的CdS-2。
（2）系列光电分析测试表明S空位的引入增强了CdS对太阳光的吸收能力，同时能够抑制其光生电子-空穴的复合，使得更多的电子参与反应；理论计算表明S空位的引入更能良好吸附反应物气体分子CO2，而镉空位的引入在该体系中不管是光电化学性质还是对反应物的吸附方面并未表现优异性能。
（3）CO2光还原性能测试结果表明，含S空位的CdS-0.25性能最佳，其产物CO、CH4、H2的生成速率分别为1.69、0.41、0.11 µmol/（g·h），比镉空位CdS-2产物分别提升了15.8、2、1.2倍。
基金
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  • 宜宾学院科技计划资助(412-2021PY091)
文献
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2026年第54卷第4期
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doi: 10.11868/j.issn.1001-4381.2024.000342
  • 接收时间：2024-05-13
  • 首发时间：2026-10-27
  • 出版时间：2026-04-20
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  • 收稿日期：2024-05-13
  • 录用日期：2024-07-01
基金
宜宾学院科技计划资助(412-2021PY091)
作者信息
    1.宜宾学院 材料与化学工程学院，四川 宜宾 644000
    2.宜宾学院 国有资产与实验设备管理处，四川 宜宾 644000

通讯作者:

郭兰（1993—），女，助教，硕士，研究方向为能源催化材料的制备与应用，联系地址：四川省宜宾市三江新区大学路5号宜宾学院二期（644000），E-mail：
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https://castjournals.cast.org.cn/joweb/clgc/CN/10.11868/j.issn.1001-4381.2024.000342
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
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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