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Article(id=1236596125973672013, tenantId=1146029695717560320, journalId=1210938733613449225, issueId=1236596124832821317, articleNumber=null, orderNo=null, doi=10.19666/j.rlfd.202408209, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1724860800000, receivedDateStr=2024-08-29, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1772757091276, onlineDateStr=2026-03-06, pubDate=1748102400000, pubDateStr=2025-05-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1772757091276, onlineIssueDateStr=2026-03-06, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1772757091276, creator=13701087609, updateTime=1772757091276, updator=13701087609, issue=Issue{id=1236596124832821317, tenantId=1146029695717560320, journalId=1210938733613449225, year='2025', volume='54', issue='5', pageStart='1', pageEnd='162', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=0, articleOrder=1, issueType=-1, specialIssue=null, createTime=1772757091004, creator=13701087609, updateTime=1772757664851, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1236598531780309922, tenantId=1146029695717560320, journalId=1210938733613449225, issueId=1236596124832821317, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1236598531780309923, tenantId=1146029695717560320, journalId=1210938733613449225, issueId=1236596124832821317, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=73, endPage=81, ext={EN=ArticleExt(id=1236596126263078992, articleId=1236596125973672013, tenantId=1146029695717560320, journalId=1210938733613449225, language=EN, title=Effects of CuO and CuCl2 additives on thermophysical properties of binary carbonate molten salts, columnId=1236596126195970127, journalTitle=Thermal Power Generation, columnName=Special topic on new power generation technology, runingTitle=null, highlight=null, articleAbstract=

Micro-nano particle doping is an important method for the modification of molten salt thermal storage materials. By taking a binary carbonate molten salt mixture of 40Li2CO3-60Na2CO3 (mass fraction) as the base molten salt, CuO and CuCl2 as the dopants, three composite molten salt phase change thermal storage materials, namely CuO-Li2CO3-Na2CO3, CuCl2-Li2CO3-Na2CO3, and CuO-CuCl2-Li2CO3-Na2CO3, were re prepared separately using a high-temperature melting method. Moreover, the thermal properties of these compounds were tested, and the effects of additives on the modification of binary carbonate molten salts and composite molten salt phase change thermal storage materials were investigated. The results show that, the melting point of the Li2CO3-Na2CO3 molten salt with 0.24% CuO addition decreased by 5.2 ℃, the latent heat of phase change decreased by 98.1 J/g, the average specific heat capacity of the solid phase decreased by 0.39 J/(g·℃), and the average specific heat capacity of the liquid phase decreased by 0.77 J/(g·℃). The upper limit of the operating temperature increased by 4 ℃. For the Li2CO3-Na2CO3-CuCl2 molten salt with 0.06% CuO addition, the melting point increased by 9.6 ℃, the latent heat of phase change decreased by 15 J/g, the average specific heat capacity of the solid phase increased by 0.07 J/(g·℃), and the average specific heat capacity of the liquid phase increased by 0.12 J/(g·℃). The upper limit of the operating temperature increased by 17 ℃. Both molten salts exhibited improved thermal conductivity performance after the addition of CuO.

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微纳颗粒掺杂是熔盐相变储热材料改性的重要方法。以40Li2CO3-60Na2CO3（质量分数）二元碳酸熔盐为基体熔盐，CuO和CuCl2作为添加剂，利用高温熔融法分别制备了CuO-Li2CO3-Na2CO3、CuCl2-Li2CO3-Na2CO3和CuO-CuCl2-Li2CO3-Na2CO3 3种复合熔盐相变储热材料，对其热物性进行了测试，研究了添加剂对二元碳酸熔盐和复合熔盐相变储热材料的改性效果。结果表明：添加质量分数0.24%CuO的Li2CO3-Na2CO3熔盐较基盐熔点下降5.2 ℃，相变潜热下降98.1 J/g，固相和液相平均比热容分别下降0.39 J/(g·℃)和0.77 J/(g·℃)，上限使用温度上升4 ℃；添加质量分数0.06%CuO的Li2CO3-Na2CO3-CuCl2熔盐较基盐熔点上升9.6 ℃，相变潜热下降15 J/g，固相和液相平均比热容分别上升0.07 J/(g·℃)和0.12 J/(g·℃)，上限使用温度上升17 ℃；2种熔盐在添加CuO后导热性能均得到提高。

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田禾青（1987），男，博士，副教授，主要研究方向为热能储存与转换技术，。

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田禾青（1987），男，博士，副教授，主要研究方向为热能储存与转换技术，。

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田禾青（1987），男，博士，副教授，主要研究方向为热能储存与转换技术，。

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Thermal stability of Li2CO3-Na2CO3 based high-temperature phase change materials[J]. Energy Storage Science and Technology, 2013, 2(4): 369-376., articleTitle=Thermal stability of Li2CO3-Na2CO3 based high-temperature phase change materials, refAbstract=null)], funds=[Fund(id=1236610620582318165, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, awardId=51906228, language=EN, fundingSource=National Natural Science Foundation of China(51906228), fundOrder=null, country=null), Fund(id=1236610620691370072, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, awardId=51906228, language=CN, fundingSource=国家自然科学基金项目(51906228), fundOrder=null, country=null), Fund(id=1236610620821393502, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, awardId=202103007, language=EN, fundingSource=Henan Postdoctoral Research Project(202103007), fundOrder=null, country=null), Fund(id=1236610620951416932, tenantId=1146029695717560320, journalId=1210938733613449225, 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figs=[ArticleFig(id=1236610618044765127, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Fig.1, caption=Schematic diagram of heat absorption performance test device, figureFileSmall=m5XNBaBlcRT2F12z2Ffgww==, figureFileBig=nXpO7Pl6PLcAXKqTwSkhCQ==, tableContent=null), ArticleFig(id=1236610618199954381, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=图1, caption=吸热性能测试装置示意, figureFileSmall=m5XNBaBlcRT2F12z2Ffgww==, figureFileBig=nXpO7Pl6PLcAXKqTwSkhCQ==, tableContent=null), ArticleFig(id=1236610618384503770, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Fig.2, caption=Properties of the Li2CO3-Na2CO3 samples modified with CuO and CuCl2, figureFileSmall=YD3uS4RBMNAZVdJLroQz+A==, figureFileBig=IUyAldvVIpm/jZWRekSYag==, tableContent=null), ArticleFig(id=1236610618602607585, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=图2, caption=CuO和CuCl2改性后的Li2CO3-Na2CO3样品特性, figureFileSmall=YD3uS4RBMNAZVdJLroQz+A==, figureFileBig=IUyAldvVIpm/jZWRekSYag==, tableContent=null), ArticleFig(id=1236610618715853799, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Fig.3, caption=Specific heat capacity of Li2CO3-Na2CO3 with different amounts of CuO addition, figureFileSmall=cymTd20oeTYOtcWy7M+6sg==, figureFileBig=s7wnqXtMksy4iIaD93kNIg==, tableContent=null), ArticleFig(id=1236610618808128495, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=图3, caption=不同CuO添加量下Li2CO3-Na2CO3的比热容, figureFileSmall=cymTd20oeTYOtcWy7M+6sg==, figureFileBig=s7wnqXtMksy4iIaD93kNIg==, tableContent=null), ArticleFig(id=1236610618904597493, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Fig.4, caption=Specific heat capacity of Li2CO3-Na2CO3 with CuCl2 addition, figureFileSmall=FF+W90Z6iNaLh6xVe0NI2A==, figureFileBig=wY53sPLylvlKhuewmh0kYQ==, tableContent=null), ArticleFig(id=1236610619038815230, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=图4, caption=添加CuCl2后Li2CO3-Na2CO3的比热容, figureFileSmall=FF+W90Z6iNaLh6xVe0NI2A==, figureFileBig=wY53sPLylvlKhuewmh0kYQ==, tableContent=null), ArticleFig(id=1236610619156254723, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Fig.5, caption=Specific heat capacity of Li2CO3-Na2CO3-CuCl2 with different amounts of CuO addition, figureFileSmall=64v58CNpjTofaAvnU70Paw==, figureFileBig=85c0uqjJgZO4kpwHKihPxA==, tableContent=null), ArticleFig(id=1236610619294666761, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=图5, 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figureFileSmall=f4eWqPf34Sd2M5dbs/IvQw==, figureFileBig=ZGqiTtY/4RzcinKqRD2l/Q==, tableContent=null), ArticleFig(id=1236610619739263005, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=图7, caption=样品吸热升温曲线, figureFileSmall=f4eWqPf34Sd2M5dbs/IvQw==, figureFileBig=ZGqiTtY/4RzcinKqRD2l/Q==, tableContent=null), ArticleFig(id=1236610619881869347, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Tab.1, caption=

Experimental materials

, figureFileSmall=null, figureFileBig=null, tableContent=
实验材料纯度生产厂家
碳酸锂（Li2CO3）98.0%国药集团化学试剂有限公司
碳酸钠（Na2CO3）99.8%国药集团化学试剂有限公司
氯化铜（CuCl2）98.0%上海麦克林生化科技股份有限公司
氧化铜（CuO）99.9%北京翠铂林有色金属技术开发中心有限公司
), ArticleFig(id=1236610619990921259, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=表1, caption=

实验材料

, figureFileSmall=null, figureFileBig=null, tableContent=
实验材料纯度生产厂家
碳酸锂（Li2CO3）98.0%国药集团化学试剂有限公司
碳酸钠（Na2CO3）99.8%国药集团化学试剂有限公司
氯化铜（CuCl2）98.0%上海麦克林生化科技股份有限公司
氧化铜（CuO）99.9%北京翠铂林有色金属技术开发中心有限公司
), ArticleFig(id=1236610620099973169, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Tab.2, caption=

The compositions of composite molten salts

, figureFileSmall=null, figureFileBig=null, tableContent=
名称Li2CO3Na2CO3CuCl2CuO
LN040.00060.00000
LN140.00060.00000.187
LN240.00060.00000.240
LNC040.00060.0003.0000
LNC140.00060.0003.0000.060
), ArticleFig(id=1236610620183859258, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=表2, caption=

复合熔盐的成分

, figureFileSmall=null, figureFileBig=null, tableContent=
名称Li2CO3Na2CO3CuCl2CuO
LN040.00060.00000
LN140.00060.00000.187
LN240.00060.00000.240
LNC040.00060.0003.0000
LNC140.00060.0003.0000.060
), ArticleFig(id=1236610620280328257, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=EN, label=Tab.3, caption=

Temperatures of the samples suffering the same heating time

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材料L0处温度L10处温度/L20处温度/
LN0420.21423.74431.26
LN2429.77432.76444.79
LNC0376.15378.23384.33
LNC1400.44411.97410.02
), ArticleFig(id=1236610620355825735, tenantId=1146029695717560320, journalId=1210938733613449225, articleId=1236596125973672013, language=CN, label=表3, caption=

样品在相同加热时间下的温度

, figureFileSmall=null, figureFileBig=null, tableContent=
材料L0处温度L10处温度/L20处温度/
LN0420.21423.74431.26
LN2429.77432.76444.79
LNC0376.15378.23384.33
LNC1400.44411.97410.02
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CuO和CuCl2添加剂对二元碳酸熔盐热物性的影响
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田禾青 , 何灿 , 郭茶秀
热力发电 | 新型发电技术专题 2025,54(5): 73-81
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热力发电 | 新型发电技术专题 2025, 54(5): 73-81
CuO和CuCl2添加剂对二元碳酸熔盐热物性的影响
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田禾青 , 何灿, 郭茶秀
作者信息
  • 郑州大学机械与动力工程学院，河南　郑州　450001

    • 田禾青（1987），男，博士，副教授，主要研究方向为热能储存与转换技术，。

Effects of CuO and CuCl2 additives on thermophysical properties of binary carbonate molten salts
Heqing TIAN , Can HE, Chaxiu GUO
Affiliations
  • School of Mechanical and Power Engineering, Zhengzhou University, Zhengzhou 450001, China
出版时间: 2025-05-25 doi: 10.19666/j.rlfd.202408209
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摘要
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微纳颗粒掺杂是熔盐相变储热材料改性的重要方法。以40Li2CO3-60Na2CO3（质量分数）二元碳酸熔盐为基体熔盐，CuO和CuCl2作为添加剂，利用高温熔融法分别制备了CuO-Li2CO3-Na2CO3、CuCl2-Li2CO3-Na2CO3和CuO-CuCl2-Li2CO3-Na2CO3 3种复合熔盐相变储热材料，对其热物性进行了测试，研究了添加剂对二元碳酸熔盐和复合熔盐相变储热材料的改性效果。结果表明：添加质量分数0.24%CuO的Li2CO3-Na2CO3熔盐较基盐熔点下降5.2 ℃，相变潜热下降98.1 J/g，固相和液相平均比热容分别下降0.39 J/(g·℃)和0.77 J/(g·℃)，上限使用温度上升4 ℃；添加质量分数0.06%CuO的Li2CO3-Na2CO3-CuCl2熔盐较基盐熔点上升9.6 ℃，相变潜热下降15 J/g，固相和液相平均比热容分别上升0.07 J/(g·℃)和0.12 J/(g·℃)，上限使用温度上升17 ℃；2种熔盐在添加CuO后导热性能均得到提高。

相变储热  /  碳酸盐  /  CuO  /  比热容  /  热稳定性

Micro-nano particle doping is an important method for the modification of molten salt thermal storage materials. By taking a binary carbonate molten salt mixture of 40Li2CO3-60Na2CO3 (mass fraction) as the base molten salt, CuO and CuCl2 as the dopants, three composite molten salt phase change thermal storage materials, namely CuO-Li2CO3-Na2CO3, CuCl2-Li2CO3-Na2CO3, and CuO-CuCl2-Li2CO3-Na2CO3, were re prepared separately using a high-temperature melting method. Moreover, the thermal properties of these compounds were tested, and the effects of additives on the modification of binary carbonate molten salts and composite molten salt phase change thermal storage materials were investigated. The results show that, the melting point of the Li2CO3-Na2CO3 molten salt with 0.24% CuO addition decreased by 5.2 ℃, the latent heat of phase change decreased by 98.1 J/g, the average specific heat capacity of the solid phase decreased by 0.39 J/(g·℃), and the average specific heat capacity of the liquid phase decreased by 0.77 J/(g·℃). The upper limit of the operating temperature increased by 4 ℃. For the Li2CO3-Na2CO3-CuCl2 molten salt with 0.06% CuO addition, the melting point increased by 9.6 ℃, the latent heat of phase change decreased by 15 J/g, the average specific heat capacity of the solid phase increased by 0.07 J/(g·℃), and the average specific heat capacity of the liquid phase increased by 0.12 J/(g·℃). The upper limit of the operating temperature increased by 17 ℃. Both molten salts exhibited improved thermal conductivity performance after the addition of CuO.

phase change thermal storage  /  carbonate salt  /  CuO  /  specific heat capacity  /  thermal stability
田禾青, 何灿, 郭茶秀. CuO和CuCl2添加剂对二元碳酸熔盐热物性的影响. 热力发电, 2025 , 54 (5) : 73 -81 . DOI: 10.19666/j.rlfd.202408209
Heqing TIAN, Can HE, Chaxiu GUO. Effects of CuO and CuCl2 additives on thermophysical properties of binary carbonate molten salts[J]. Thermal Power Generation, 2025 , 54 (5) : 73 -81 . DOI: 10.19666/j.rlfd.202408209
正文
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储能技术是解决能源供需不匹配问题的重要途径，储热技术作为其重要的组成部分在太阳能热利用、余热回收、建筑供暖等领域有广泛应用[1-5]。尤其对于聚光式太阳能发电（concentrated solar power，CSP），储热技术可以有效地解决太阳能在时间和空间上供需不匹配的问题，为发电系统提供调峰功能，在提高能源利用率和环境保护方面具有重要的意义[6-10]。其中，熔盐是重要的中高温相变储热材料。熔盐是无机盐的熔融体，具有较高的相变潜热和稳定性、较宽范围内的低蒸汽压、较低的黏度和成本等特性，使其在CSP技术中具有良好的发展前景[11-16]。在CSP技术中，常用的熔盐储热介质包括硝酸熔盐、氯化物熔盐、氟化物熔盐和碳酸熔盐[17]。由于具有比热容较高、热稳定性好、且腐蚀性小等一系列优势，碳酸熔盐成为新一代CSP系统中的潜在储热材料。
为了满足新一代CSP技术对熔盐性能的需求，需要进一步提高熔盐的热物性。目前熔盐热物性的改性方法之一为掺杂纳米颗粒形成熔盐基纳米流体[18]。纳米颗粒常用材料为金属及金属氧化物、无机非金属（如碳化物和氮化物）和碳材料（如石墨、石墨烯和碳纳米管）等。研究表明，纳米颗粒的添加量、粒径大小和分散度等因素均对熔盐的改性效果有显著影响[19-21]。Wang等人[22]对Hitec盐掺杂了不同质量分数的纳米TiO2颗粒，并对复合储热材料的热物性进行了表征。研究发现，掺杂纳米TiO2颗粒后Hitec盐的性能得到了提升，其中添加粒径25 nm、质量分数0.062 5%的复合熔盐相比于原熔盐比热容和导热系数分别提高了12%和15%。Zhang等人[23]利用两步水溶液法制备了3种粒径纳米Al2O3颗粒掺杂的Li2CO3-Na2CO3-K2CO3复合熔盐材料，并实验测量了其热物性。结果表明，粒径20 nm、掺杂质量分数1%的复合熔盐材料改性效果最好，其固相和液相平均比热容分别提高了18.5%和33%，导热提高了23.3%，适合作为未来CSP系统中的储热材料。Yang等人[24]在三元碳酸熔盐Li2CO3-Na2CO3-K2CO3中掺杂质量分数1%~5%的纳米ZnO颗粒。研究表明，添加质量分数1.0%、粒径30 nm ZnO纳米颗粒的复合碳酸熔盐改性效果最好，平均固态和液态比热容分别提高了16.56%和21.61%。Yu等人[25]通过对二元硝酸熔盐（NaNO3-KNO3）/EG复合相变材料掺杂不同质量分数的SiO2纳米颗粒研究其热物性的变化。结果表明，当添加质量分数1% SiO2纳米颗粒，熔盐材料的平均比热容、平均热扩散系数以及热导率达到最大值，分别为3.92 J/(g·K)、1.64 mm2/s和8.47 W/(m·K)，热物性有明显提升。Xiong等人[26]通过对Li2CO3-K2CO3分别掺杂质量分数1.0%的MgO和SiO2纳米颗粒，发现改性后熔盐比热容相比基盐分别提升27.5%~34.1%和11.0%~20.7%。Duan等人[27]为提高HTS熔盐导热系数，添加不同质量分数的改性天然石墨，发现添加质量分数25%改性天然石墨时熔盐导热系数由0.76 W/(m·K)提高至11.26 W/(m·K)，但比热容会降低。
添加可溶性的添加剂也是熔盐改性的方法之一[18]，其是指在基体熔盐中添加一种或者多种能溶于基体熔盐的其他种类物质，从而形成复合熔盐来实现熔盐改性的效果。Wan等人[28]将Na2CO3作为添加剂加入至Solar Salt中测试改性效果，结果表明，添加质量分数1% Na2CO3就能使Solar Salt的工作温度范围扩大20 ℃，稳定性提高3.2%。Shen等人[29]在47Ca(NO3)2-53KNO3（质量分数，下同）熔盐中添加2种新型添加剂拓宽了其工作温度范围，凝固点和分解温度分别达到135.2 ℃和639.1 ℃。少量的添加剂就能显著改变熔盐的热物性，某些添加剂还能与熔盐中的组分发生化学反应改变熔盐物质组成及熔体结构。
综上，在熔盐储热材料中掺杂纳米颗粒或者添加可溶性添加剂可以有效改善熔盐的热物性，但是目前对于同时掺杂纳米颗粒和添加剂的研究较少，同时对掺杂后熔盐热物性的改性效果也不明确。鉴于此，本研究以二元碳酸熔盐作为基体熔盐，CuO纳米颗粒和CuCl2添加剂作为改性材料，利用高温熔融法制备了CuO和CuCl2掺杂的复合碳酸熔盐储热材料，分析了纳米颗粒和添加剂对熔盐热物性的改性效果，为纳米颗粒和添加剂掺杂改性熔盐热物性的研究提供了理论基础与参考。
1　材料和方法
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1.1　样品制备
1.1.1　实验材料
本文选择40Li2CO3-60Na2CO3二元共晶碳酸熔盐作为基体熔盐储热材料，CuO颗粒和CuCl2作为添加剂改善熔盐热物性。实验所用到的材料见表1。
1.1.2　实验设备
实验中使用的设备为箱式电阻炉（天津市泰斯特仪器有限公司SRJX-8-13D）、井式电阻炉（上海意丰电炉有限公司YFFG70X195/10Q）、电动搅拌机（上海垒固仪器有限公司GZ120-S）、数据采集仪（是德科技有限公司34972A）和电热鼓风干燥箱（天津市泰斯特仪器有限公司WGL-45B）。
1.1.3　样品制备
采用高温熔融法制备Li2CO3-Na2CO3二元碳酸熔盐。首先，根据共晶成分比例准确称量Li2CO3和Na2CO3 2种熔盐，均匀混合后放入刚玉坩埚内；然后，将坩埚放入箱式电阻炉内加热熔化。初始温度设定为50 ℃，以5 ℃/min的加热速率升温至800 ℃，在800 ℃保温2 h待熔盐充分熔化，再以5 ℃/min的速率降温至600 ℃，保温0.5 h确保完全形成低共熔点混合物。保温结束后，取出熔盐倒入不锈钢托盘中自然冷却至室温。取出凝固后的熔盐研磨成粉末，放入电热鼓风干燥箱内烘干备用。
同样采用高温熔融法制备Li2CO3-Na2CO3-CuCl2复合熔盐。首先，将质量分数97%的Li2CO3-Na2CO3与质量分数3%的CuCl2均匀混合于刚玉坩埚内，以5 ℃/min的加热速率从室温升温至750 ℃；然后，按照前述保温流程操作确保熔盐完全融化，保温结束后倒入不锈钢托盘中待其自然冷却；最后，将熔盐研磨成粉末并烘干备用。
称取150 g预制备的Li2CO3-Na2CO3（或Li2CO3-Na2CO3-CuCl2）熔盐置入刚玉坩埚中，然后放入井式炉内以5 ℃/min的升温速率从50 ℃加热至750 ℃后保温。保温1 h使熔盐充分熔化后，添加CuO至熔体中，并以100 r/min的搅拌速度搅拌5 h使其均匀分散，取出坩埚将复合熔盐倒入宽口径不锈钢盘冷却，将凝固后的熔盐研磨成粉末，即可得到CuO-Li2CO3-Na2CO3（或CuO-Li2CO3-Na2CO3-CuCl2）复合熔盐材料。
1.2　实验方法
1.2.1　差式扫描量热法
通过差式扫描量热法测试得到样品的比热容、熔点及相变潜热等信息。具体的测试条件为将样品从室温以10 ℃/min的升温速率先升温至200 ℃，保温0.5 h去除吸附水后再继续以10 ℃/min的升温速率升温至800 ℃。
1.2.2　热重分析
为了测量样品的上限使用温度，利用PerkinElmer同步热分析仪STA8000-Frontier分析测量熔盐样品的质量损失曲线。整个测试过程在空气氛围中进行，且样品使用带盖的氧化铝坩埚盛装。以10 ℃/min的升温速率从室温升温至200 ℃，保温30 min除去样品中水分，接着继续以10 ℃/min升温至1 000 ℃，测试结束后得到样品质量随温度的变化曲线，确定其上限使用温度。
1.2.3　吸热性能
在受到同一热源的加热过程中，由于导热性能的不同，添加不同微纳米颗粒的熔盐材料在同一部位的温度上升速度不同。通过测量加热过程中样品的温度随时间的变化曲线研究样品的导热性能。首先，每次称取一定质量的熔盐样品至坩埚，并放入井式电阻炉中；然后，启动数据采集仪，将3根K型测温热电偶与数据采集仪连接，再将3根热电偶插入粉末状熔盐堆心部，启动数据采集仪并等待数据采集仪采集5 min，观察仪器测量温度确认其连接稳定并保证热电偶与熔盐之间达到热平衡。在本实验中用到的坩埚半径为30 mm，选取3根热电偶的位置分别放置在坩埚心部、距离心部10 mm处、距离心部20 mm处，吸热性能测试装置如图1所示。
准备完成后打开电阻炉以6.5 ℃/min的加热功率将熔盐升温至750 ℃，记录坩埚内熔盐在升温过程的温度变化。完成记录后，将热电偶取出冷却后清理干净，并将熔化后的熔盐倒入不锈钢盘中冷却后装袋回收。
2　结果与讨论
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本文将掺杂质量分数0、0.187%和0.240% CuO的Li2CO3-Na2CO3二元熔盐样品分别命名为LN0、LN1和LN2，将添加质量分数3.000% CuCl2的Li2CO3-Na2CO3复合熔盐命名为LNC0，将掺杂质量分数0.060% CuO的Li2CO3-Na2CO3-CuCl2的复合熔盐命名为LNC1，具体见表2。
2.1　熔点及相变潜热
二元碳酸熔盐和复合熔盐的DSC曲线如图2a)所示，熔点和相变潜热的变化如图2b)所示，熔点均为起始熔化温度。由图2a)可知，纯二元碳酸熔盐LN0的熔点为507.7 ℃，加入CuO后的二元碳酸熔盐熔点略微减小，其中LN1和LN2的熔点分别为499.9 ℃和502.4 ℃，较纯盐分别下降了7.8 ℃和5.3 ℃，可认为少量CuO掺杂对熔盐熔点没有影响。LN0、LN1和LN2的相变潜热分别为513.9、437.8、415.8 J/g，LN1和LN2相较于LN0分别下降了76.1、98.1 J/g，可能的原因是：CuO的掺杂可能会破坏熔盐的晶格结构，使被破坏部位周围的原子更加活跃，原子会变得更容易吸收热量和更容易熔化，使相变潜热减小；另一方面CuO的熔点为1 446 ℃，远高于熔盐的熔点，在研究温度条件下CuO占据了熔盐总体的份额但是没有发生熔化产生相变潜热。因此，CuO的掺杂使复合熔盐材料的相变潜热降低，且掺杂量越大，复合熔盐的相变潜热越低。
在二元碳酸熔盐中加入质量分数3%的CuCl2改性后，复合熔盐LNC0的熔点为464.2 ℃，熔点较原二元碳酸熔盐LN0降低了43.5 ℃，相变潜热降至272.4 J/g。研究发现CuCl2会在高温下与Na2CO3反应生成了CuCO3与NaCl，NaCl的熔点与相变潜热均比Na2CO3低，导致复合熔盐LNC0的熔点降低，潜热储热能力下降。
在Li2CO3-Na2CO3-CuCl2复合熔盐中掺杂CuO后，复合熔盐LNC1的熔点为473.8 ℃，相变潜热为257.4 J/g。相较于原二元碳酸熔盐LN0，熔点降低了33.9 ℃，相变潜热降低了256.5 J/g；相较于添加CuCl2改性后的复合熔盐LNC0，熔点升高了9.6 ℃，相变潜热下降了15 J/g。
2.2　比热容
图3为不同CuO添加量下二元碳酸熔盐的固相比热容和液相比热容随温度的变化情况。在固相区（250~450 ℃），所有样品的比热容随着温度的升高而增大，且温度在360~370 ℃区间时出现了突变，文献[30]表明Li2CO3-Na2CO3二元熔盐的主要共晶成分LiNaCO3在360 ℃时发生了从β相到γ相的固-固转变，物质结构的变化会对其比热容产生影响。通过计算可得，在250~350 ℃温度区间，LN0、LN1和LN2的固相平均比热容分别为1.87、1.70、1.48 J/(g·℃)，LN1与LN2的平均固相比热容相比于LN0降低了0.17、0.39 J/(g·℃)。在液相区（575~750 ℃），LN0、LN1和LN2的液相平均比热容分别为2.43、2.22、1.66 J/(g·℃)，LN1与LN2的平均液相比热容较LN0分别降低了0.21、0.77 J/(g·℃)。可知，在研究的添加量范围内，二元碳酸熔盐的比热容随CuO添加量的增大而减小。金属氧化物颗粒的分散稳定性是制约熔盐纳米流体比热强化的关键因素，随CuO添加量的增大，CuO在熔盐中发生了团聚，使其比表面积减小，且影响熔盐内半固态层的产生，因此降低了比热容。
图4为添加CuCl2后Li2CO3-Na2CO3的比热容对比。在固相区（250~350 ℃），LN0和LNC0的固相平均比热容分别为1.87、1.35 J/(g·℃)，添加CuCl2后平均固相比热容下降了0.52 J/(g·℃)。在液相区（575~750 ℃），LN0和LNC0的液相平均比热容分别为2.43、1.64 J/(g·℃)，添加CuCl2后平均液相比热容下降了0.79 J/(g·℃)。添加剂CuCl2在高温下与Na2CO3反应生成CuCO3与NaCl，在相同温度下NaCl的比热容比Na2CO3低，因此添加CuCl2后使二元碳酸熔盐比热容减小。
图5为不同CuO添加量下Li2CO3-Na2CO3-CuCl2复合熔盐材料的固相比热容和液相比热容随温度的变化情况。同样的，温度在360~370 ℃区间时比热容出现了突变，原因同上分析。在250~350 ℃温度区间，LNC0和LNC1的固相平均比热容分别为1.35、1.42 J/(g·℃)，LNC1的固相比热容较LNC0上升了0.07 J/(g·℃)。在液相区（550~750℃），LNC0和LNC1的液相平均比热容分别为1.64、1.76 J/(g·℃)，LNC1的平均液相比热容较LNC0上升了0.12 J/(g·℃)。因此掺杂了CuO后复合熔盐整体的比热容增大了，原因与二元碳酸熔盐相反，认为CuCl2的添加有利于CuO的稳定分散，形成半固态层。
2.3　热稳定性
采用热重分析了CuO-Li2CO3-Na2CO3复合熔盐及CuO-Li2CO3-Na2CO3-CuCl2复合熔盐的上限使用温度，规定样品质量损失5%时的温度即为样品的上限使用温度。图6对比了添加CuCl2和CuO前后复合熔盐的质量损失曲线。由图6可知，掺杂CuO后，二元碳酸熔盐的高温热稳定性和上限使用温度均得到了提高。在温度827 ℃前，LN2的质量损失比LN0的质量损失更快，在此之后LN2样品的热稳定性更好。当2个样品质量损失均达到5%时，LN0和LN2的温度分别为843.5、847.3 ℃。
添加质量分数3%的CuCl2后，二元碳酸熔盐的热稳定性和上限使用温度均降低。但LN0和LNC0在温度500 ℃前依然能保持性能稳定，无质量变化。当温度为830 ℃时，LNC0质量损失达到5%。和原二元碳酸熔盐相比，LNC0的上限使用温度降低了13.5 ℃。
同时在Li2CO3-Na2CO3熔盐中掺杂CuO和CuCl2后，形成的复合熔盐LNC1同样能在温度500 ℃前能保持稳定，质量没有改变。随着温度的升高，LNC1从温度520 ℃时开始发生失重现象，在其上限使用温度847 ℃时质量损失达到5%。可知，随着温度的升高，同温度下LNC1的质量损失低于LNC0，表明CuO的掺杂增强了LNC0的热稳定性；与原二元碳酸熔盐LN0相比，在温度800 ℃后，LNC1的质量损失量低于LN0，表明同时掺杂CuO和CuCl2增强了原二元碳酸熔盐的高温热稳定性；与单纯掺杂CuO的LN2相比，在温度844 ℃前，LNC1的质量损失量低于LN2，表明CuO和CuCl2的同时掺杂增强了其热稳定性。但在温度844 ℃后LNC1的热稳定性不如LN2。综上，可溶性添加剂CuCl2的添加降低了熔盐的热稳定性和上限使用温度，而CuO的掺杂则可以提高二元碳酸熔盐的热稳定性。
2.4　吸热性能
通过恒定加热速率下不同位置处样品的吸热升温过程的温度变化评定样品的吸热性能，具体如图7所示。
由图7可知，由于为周向环形加热，距离坩埚边缘越近，升温越早。其中，距心部20 mm（L20）、距心部10 mm（L10）、心部（L0）3个位置处在升温50 min后的温度见表3。
由表3可知，升温50 min时，LN0样品在L20、L10和L0 3个位置处的温度分别为431.26、423.74、420.21 ℃，LN2样品在这3个位置的温度分别为444.79、432.76、429.77 ℃，LNC0样品在这3个位置的温度分别为384.33、378.23、376.15 ℃，LNC1样品在这3个位置的温度分别为410.02、411.97、400.44 ℃。升温50 min后，不同位置处的温度遵循LN2˃LN0˃ LNC1˃ LNC0。在相同初始温度、升温速率与加热时间的条件下，温度变化越大代表热量传递的速度就越快，吸热能力更强，间接反映4种材料导热性能的强弱：LN2˃LN0˃LNC1˃ LNC0。综上，掺杂CuO后，二元碳酸熔盐与复合碳酸熔盐的导热性能和吸热能力均得到了强化。但添加可溶性添加剂CuCl2后，二元碳酸盐的导热性能和吸热性能反而减弱。
3　结论
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本文使用高温熔融法将CuO和CuCl2分别掺杂在Li2CO3-Na2CO3二元碳酸熔盐中，制备了CuO-Li2CO3-Na2CO3、CuCl2-Li2CO3-Na2CO3和CuO-CuCl2-Li2CO3-Na2CO3复合碳酸熔盐。采用DSC法测试了二元碳酸熔盐和3种复合熔盐的熔点、相变潜热和比热容，利用TG法研究了其热稳定性和上限使用温度，运用步热实验分析了其吸热性能，主要研究结论如下。
1）添加CuO后，二元碳酸熔盐的熔点几乎不变，但其相变潜热和比热容均随CuO添加量的增大而减小。添加CuCl2后，二元碳酸熔盐的熔点、相变潜热和比热容均下降。CuO的掺杂几乎未改变CuCl2-Li2CO3-Na2CO3复合熔盐的熔点，但其相变潜热随CuO的添加而减小，比热容随CuO的添加而增加。
2）CuO的掺杂增加了二元碳酸熔盐的热稳定性和上限使用温度，而CuCl2的添加减少了二元碳酸盐的热稳定性和上限使用温度。添加质量分数3% CuCl2后，二元碳酸盐的上限使用温度下降13.5 ℃。添加质量分数0.24%和0.06% CuO后，二元碳酸熔盐和CuCl2-Li2CO3-Na2CO3复合熔盐的上限使用温度分别上升4 ℃和17 ℃。
3）掺杂CuO后，二元碳酸熔盐和CuCl2-Li2CO3-Na2CO3复合熔盐的吸热性能均得到增强，但CuCl2的添加使二元碳酸熔盐吸热性能减弱。以6.5 ℃/min的速率升温50 min时，LNC1和LN2熔盐的心部温度较原熔盐分别增加了24.29 ℃和9.56 ℃，而LNC0熔盐的心部温度较LN0降低了44.06 ℃。
基金
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  • 国家自然科学基金项目(51906228)
  • 河南省博士后项目(202103007)
文献
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2025年第54卷第5期
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doi: 10.19666/j.rlfd.202408209
  • 接收时间：2024-08-29
  • 首发时间：2026-03-06
  • 出版时间：2025-05-25
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  • 收稿日期：2024-08-29
基金
National Natural Science Foundation of China(51906228)
国家自然科学基金项目(51906228)
Henan Postdoctoral Research Project(202103007)
河南省博士后项目(202103007)
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    郑州大学机械与动力工程学院，河南　郑州　450001
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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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