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Article(id=1199642730042327060, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199642729207660562, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2023.11.005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1669046400000, receivedDateStr=2022-11-22, revisedDate=1677081600000, revisedDateStr=2023-02-23, acceptedDate=null, acceptedDateStr=null, onlineDate=1763946715125, onlineDateStr=2025-11-24, pubDate=1700409600000, pubDateStr=2023-11-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763946715125, onlineIssueDateStr=2025-11-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763946715125, creator=13701087609, updateTime=1763946715125, updator=13701087609, issue=Issue{id=1199642729207660562, tenantId=1146029695717560320, journalId=1149653034449285133, year='2023', volume='56', issue='11', pageStart='1', pageEnd='116', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1763946714927, creator=13701087609, updateTime=1766563708953, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210619197772657229, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199642729207660562, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210619197772657230, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1199642729207660562, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=28, endPage=34, ext={EN=ArticleExt(id=1199642730340122645, articleId=1199642730042327060, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and electrical property study of black shale/HDPE composite, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

To investigate the possibility of using black shale as a filler in the plastic industry, the composition and morphology of black shale in Guilin area were studied. It was found that black shale has nano layered structure, and was mainly composed of silica, K-feldspar, and organic carbon. The black shale/HDPE composite were prepared by modifying black shale with different coupling agents and surfactants, and their mechanical properties, morphology, volume resistivity, and dielectric constant were studied. The results show that aluminate coupling agent and sodium dodecylbenzene sulfonate can improve the compatibility between shale and HDPE. When the shale filling amount is 50 phr, the tensile strength, impact strength, and volume resistivity of black shale/HDPE composite reduce. The tensile strength remains at 23.47 MPa, the maximum impact strength is 6.39 kJ/m2, and the volume resistivity can also be maintained above 1014 Ω·cm, maintaining good mechanical properties and insulating properties.

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为了研究黑色页岩作为填料应用于塑料工业的可能性，本文对桂林地区的黑色页岩进行了成分和形貌研究，发现其为纳米层状结构，主要由二氧化硅、钾长石及有机碳组成。利用不同的偶联剂与表面活性剂改性黑色页岩，制备了黑色页岩/HDPE复合材料，并对其力学性能、形貌、体积电阻率和介电常数进行了研究。结果表明：铝酸酯偶联剂与十二烷基苯磺酸钠能够改善页岩与HDPE之间的相容性，当页岩填充量为50份时，黑色页岩/HDPE复合材料的拉伸强度、冲击强度和体积电阻率有所降低，拉伸强度仍保持在23.47 MPa，冲击强度最高为6.39 kJ/m2，体积电阻率也可维持在1014 Ω·cm以上，保持了较好的力学性能和绝缘性能。

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邓卫星（1981-），男（汉族），安徽淮北人，高级实验师，主要从事高分子复合材料的研究。
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韩松（1994-），男（汉族），山东临沂人，硕士生，主要从事高分子复合材料的研究。

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韩松（1994-），男（汉族），山东临沂人，硕士生，主要从事高分子复合材料的研究。

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韩松（1994-），男（汉族），山东临沂人，硕士生，主要从事高分子复合材料的研究。

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份数/份拉伸强度/MPa
ACA+CTABACA+SDBSKH560+CTABKH560+OTABKH560+SDS
523.8924.0624.0124.4124.12
1023.3723.9623.8323.8924.02
1523.3523.9323.7524.1324.01
2023.1223.8523.5923.4023.80
2523.1023.8523.5623.4723.72
3023.0423.7123.3823.3023.65
3522.9123.4923.2022.6223.37
4022.4823.4523.1822.3923.26
4522.3723.1623.0522.2923.07
5022.1623.4723.1722.3922.71
), ArticleFig(id=1217475522741846028, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199642730042327060, language=CN, label=表1, caption=

黑色页岩/HDPE复合材料的拉伸强度

, figureFileSmall=null, figureFileBig=null, tableContent=
份数/份拉伸强度/MPa
ACA+CTABACA+SDBSKH560+CTABKH560+OTABKH560+SDS
523.8924.0624.0124.4124.12
1023.3723.9623.8323.8924.02
1523.3523.9323.7524.1324.01
2023.1223.8523.5923.4023.80
2523.1023.8523.5623.4723.72
3023.0423.7123.3823.3023.65
3522.9123.4923.2022.6223.37
4022.4823.4523.1822.3923.26
4522.3723.1623.0522.2923.07
5022.1623.4723.1722.3922.71
), ArticleFig(id=1217475522825732112, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199642730042327060, language=EN, label=Tab.2, caption=The impact strength of black shale/HDPE composite, figureFileSmall=null, figureFileBig=null, tableContent=
份数/份冲击强度/(kJ/m2)
ACA+CTABACA+SDBSKH560+CTABKH560+OTABKH560+SDS
57.207.755.627.026.80
107.187.565.687.057.00
156.867.434.786.737.02
206.807.045.175.996.37
256.606.985.235.277.13
306.407.105.655.185.74
356.226.485.605.816.47
405.586.255.685.305.15
455.346.115.144.885.77
505.286.395.234.754.94
), ArticleFig(id=1217475523043835921, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199642730042327060, language=CN, label=表2, caption=

黑色页岩/HDPE复合材料的冲击性能

, figureFileSmall=null, figureFileBig=null, tableContent=
份数/份冲击强度/(kJ/m2)
ACA+CTABACA+SDBSKH560+CTABKH560+OTABKH560+SDS
57.207.755.627.026.80
107.187.565.687.057.00
156.867.434.786.737.02
206.807.045.175.996.37
256.606.985.235.277.13
306.407.105.655.185.74
356.226.485.605.816.47
405.586.255.685.305.15
455.346.115.144.885.77
505.286.395.234.754.94
), ArticleFig(id=1217475523190636566, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199642730042327060, language=EN, label=Tab.3, caption=The volume resistivity of black shale/HDPE composite, figureFileSmall=null, figureFileBig=null, tableContent=
份数/份体积电阻率/(Ω·cm)
ACA+CTABACA+SDBSKH560+CTABKH560+OTABKH560+SDS
51.60×10162.58×10164.08×10163.46×10163.36×1016
251.34×10152.88×10162.68×10162.20×10151.12×1016
504.73×10142.41×10151.58×10157.11×10141.77×1015
), ArticleFig(id=1217475523270328346, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1199642730042327060, language=CN, label=表3, caption=

黑色页岩/HDPE复合材料的体积电阻率

, figureFileSmall=null, figureFileBig=null, tableContent=
份数/份体积电阻率/(Ω·cm)
ACA+CTABACA+SDBSKH560+CTABKH560+OTABKH560+SDS
51.60×10162.58×10164.08×10163.46×10163.36×1016
251.34×10152.88×10162.68×10162.20×10151.12×1016
504.73×10142.41×10151.58×10157.11×10141.77×1015
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黑色页岩/HDPE复合材料的制备及电性能研究
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韩松 1 , 彭锦雯 1 , 黎玲 2 , 容北国 2 , 刘远立 1 , 邓卫星 1, 3
绝缘材料 | 材料研究 2023,56(11): 28-34
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绝缘材料 | 材料研究 2023, 56(11): 28-34
黑色页岩/HDPE复合材料的制备及电性能研究
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韩松1, 彭锦雯1, 黎玲2, 容北国2, 刘远立1, 邓卫星1, 3
作者信息
  • 1桂林理工大学 材料科学与工程学院，广西 桂林 541004
  • 2桂林鸿程矿山设备制造有限公司， 广西 桂林 541000
  • 3桂林师范高等专科学校 化学与药学系，广西 桂林 541000

    • 韩松（1994-），男（汉族），山东临沂人，硕士生，主要从事高分子复合材料的研究。

通讯作者:

邓卫星（1981-），男（汉族），安徽淮北人，高级实验师，主要从事高分子复合材料的研究。
Preparation and electrical property study of black shale/HDPE composite
Song HAN1, Jinwen PENG1, Ling LI2, Beiguo RONG2, Yuanli LIU1, Weixing DENG1, 3
Affiliations
  • 1College of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, China
  • 2Guilin Hongcheng Mining Equipment Manufacture Co., Ltd., Guilin 541000, China
  • 3Department of Chemistry and Pharmacy, Guilin Normal College, Guilin 541000, China
出版时间: 2023-11-20 doi: 10.16790/j.cnki.1009-9239.im.2023.11.005
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摘要
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为了研究黑色页岩作为填料应用于塑料工业的可能性，本文对桂林地区的黑色页岩进行了成分和形貌研究，发现其为纳米层状结构，主要由二氧化硅、钾长石及有机碳组成。利用不同的偶联剂与表面活性剂改性黑色页岩，制备了黑色页岩/HDPE复合材料，并对其力学性能、形貌、体积电阻率和介电常数进行了研究。结果表明：铝酸酯偶联剂与十二烷基苯磺酸钠能够改善页岩与HDPE之间的相容性，当页岩填充量为50份时，黑色页岩/HDPE复合材料的拉伸强度、冲击强度和体积电阻率有所降低，拉伸强度仍保持在23.47 MPa，冲击强度最高为6.39 kJ/m2，体积电阻率也可维持在1014 Ω·cm以上，保持了较好的力学性能和绝缘性能。

黑色页岩  /  高密度聚乙烯  /  拉伸强度  /  冲击强度

To investigate the possibility of using black shale as a filler in the plastic industry, the composition and morphology of black shale in Guilin area were studied. It was found that black shale has nano layered structure, and was mainly composed of silica, K-feldspar, and organic carbon. The black shale/HDPE composite were prepared by modifying black shale with different coupling agents and surfactants, and their mechanical properties, morphology, volume resistivity, and dielectric constant were studied. The results show that aluminate coupling agent and sodium dodecylbenzene sulfonate can improve the compatibility between shale and HDPE. When the shale filling amount is 50 phr, the tensile strength, impact strength, and volume resistivity of black shale/HDPE composite reduce. The tensile strength remains at 23.47 MPa, the maximum impact strength is 6.39 kJ/m2, and the volume resistivity can also be maintained above 1014 Ω·cm, maintaining good mechanical properties and insulating properties.

black shale  /  HDPE  /  tensile strength  /  impact strength
韩松, 彭锦雯, 黎玲, 容北国, 刘远立, 邓卫星. 黑色页岩/HDPE复合材料的制备及电性能研究. 绝缘材料, 2023 , 56 (11) : 28 -34 . DOI: 10.16790/j.cnki.1009-9239.im.2023.11.005
Song HAN, Jinwen PENG, Ling LI, Beiguo RONG, Yuanli LIU, Weixing DENG. Preparation and electrical property study of black shale/HDPE composite[J]. Insulating Materials, 2023 , 56 (11) : 28 -34 . DOI: 10.16790/j.cnki.1009-9239.im.2023.11.005
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0 引言
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高分子聚合物材料因其具有较高的体积电阻率和优良的介电性能等天然优势，被广泛应用于高压直流电缆外皮、开关插座和插线板等民用和工业电气绝缘领域，尤其是价格低廉、化学稳定性高和易加工的聚乙烯材料等[1-5]。考虑到材料成本节约和不同应用环境对聚合物材料电气绝缘性能的要求不同等因素，通常会采用填充无机填料的方法对聚合物材料进行改性，以制备复合材料[6-11]。
目前，使用的无机填料通常为碳酸钙、滑石、蒙脱土和炭黑等[9]。李长明等[6]采用蒙脱土填充聚乙烯树脂制备了复合材料，并研究了复合材料的体积电阻率和电气强度等性能，结果表明蒙脱土的加入，使复合材料中引入了更多的陷阱能级，改善了载流子浓度和迁移率，提升了复合材料的耐电老化性能。O E GOUDA等[7]采用K10黏土和高密度聚乙烯（HDPE）制备了纳米黏土/HDPE复合材料，并在200 Hz～2 MHz的高频范围内研究复合材料的相对介电常数和介质损耗因数等电性能，结果表明填料质量分数为6%时，复合材料的绝缘电阻和电气强度最佳。
伴随着矿山资源被大量开发，导致环境被严重破坏。随着人们环保意识不断增强，我国环保法规日益完善，碳酸钙、滑石、蒙脱土等无机填料的开采面临环境可持续发展的巨大压力。黑色页岩是沉积地壳中广泛存在的一种岩石组合，主要是在缺氧或贫氧条件下形成的黑色细粒泥质岩层，富含有机质和分散状硫化矿物[7]。我国西南地区的黑色页岩多暴露于地表或很薄的土层下面，在温湿气候条件下易形成具有较强腐蚀性的酸性环境[11]，如果将其合理地、科学地加工，有望代替或部分代替碳酸钙、滑石粉等填料。且黑色页岩资源丰富、价格低廉，利用黑色页岩代替传统填料，不仅可以显著降低橡塑制品的成本，而且开采后加以复垦修复能够减少环境灾害[12]。
近年来随着页岩油气的开发，裂解油页岩渣得到关注和研究[13-17]。然而黑色页岩的研究较为滞后，我国的页岩因富含有机碳，多被用来制做页岩砖，起到节约燃料的作用，但浪费了页岩资源[18]。马滨等[12]对页岩进行了原位改性，利用在天然橡胶中预先混入的硬脂酸，通过混炼过程对黑色页岩进行原位改性制备了黑色页岩粉与炭黑复合填充的天然橡胶，结果表明用10份硬脂酸原位改性的黑色页岩粉与20份炭黑复合填充的天然橡胶表现出优异的拉伸性能和耐老化性能。
关于黑色页岩作为填料对HDPE力学性能和电性能的影响尚未开展任何研究，本文对桂林地区的黑色页岩基本构成及结构进行研究，首次利用偶联剂与表面活性剂修饰制备黑色页岩/HDPE复合材料，研究偶联剂和阴阳离子表面活性剂对复合材料力学性能和电性能的影响。
1 试验
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1.1 主要原材料
高密度聚乙烯（HDPE，牌号为DMDA-8008），中国石油天然气股份有限公司独山子石化分公司；黑色页岩（粒径为10 μm），桂林鸿程矿山设备制造有限公司；抗氧剂1076、聚乙烯蜡（Luwax®A，分子量为7 000 g/mol），BASF公司；硬脂酸（SA）、十六烷基三甲基溴化铵（CTAB）、十八烷基三甲基溴化铵（OTAB）、十二烷基硫酸钠（SDS）、十二烷基苯磺酸钠（SDBS）、铝酸酯偶联剂（ACA-DL411）、γ-缩水甘油醚氧丙基三甲氧基硅烷（KH560），西陇科学有限公司。
1.2 材料制备
将黑色页岩、树脂基体、助剂以20∶1∶1的质量比在120℃条件下用高速混合机混合20 min，按照不同的偶联剂与活性剂的组合共分为5组：(a)ACA+CTAB、(b)ACA+SDBS、(c)KH560+CTAB、(d)KH560+OTAB、(e)KH560+SDS。混合均匀后的原料用双螺杆挤出机进行挤出造粒，挤出机螺杆转速为130 r/min，分段式温度分别设定为140、145、150、155、160、160、160、160、160、170℃。将制备的5组复合材料颗粒放入烘箱，设定温度为70℃烘干4 h。烘干后的颗粒用立式注塑机制备样条，注塑压力为7～9 MPa，料筒分段式温度分别设定为170、170、170、180℃。制备的样条在室温下放置24 h后进行相关测试。
1.3 测试与表征
拉伸强度利用深圳三思纵横科技股份有限公司生产的UTM4503SLXY型电子万能试验机进行测试，测试方法按照GB/T 1040.2—2006相关要求进行，拉伸速度为50 mm/min；冲击强度利用深圳三思纵横科技股份有限公司生产的PTM7000型塑料摆锤冲击试验机进行测试，测试方法按照GB/T 1843—2008相关要求进行，样条为A型缺口，摆锤能量为2.75 J；热分解行为利用德国耐驰公司生产的STA-449F5型综合热分析仪进行测试，氮气氛围，升温速率为10℃/min，测试温度为50～800℃；复合材料的断面形貌利用日立高新技术公司生产的S-4800型场发射扫描电子显微镜进行测试，将样条采用液氮低温处理后迅速折断得到脆性断裂断面，对断面进行喷金处理；复合材料的熔融指数按照GB/T 1845—2016相关要求，利用承德市科承试验机有限公司生产的XNR-400型熔体流动速率测定仪进行测试，压锤质量为2.16 kg，温度为190℃，刮料间隔为5 s；体积电阻率采用上海第六电表厂生产的PC68型高阻计进行测量；介电常数采用安捷伦公司生产的4294A型阻抗分析仪进行测试；黑色页岩粉末元素组成利用美国热电公司生产的ESCALAB 250Xi型X射线光电子能谱仪进行测定；黑色页岩粉末的XRD图谱利用荷兰帕纳公司生产的X’Pert PRO型X射线衍射仪进行测试，扫描范围为5°～80°；黑色页岩粉末的红外光谱采用KBr压片法，利用美国热电公司生产的Thermo Nexux 470型红外光谱仪进行测试。
2 结果与讨论
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2.1 黑色页岩成分组成及形貌研究
通过XRD、FTIR、TG、XPS、SEM以及EDS对黑色页岩的组成及形貌进行研究。图1为黑色页岩粉末的XRD，从图中可以看出衍射峰与PDF数据库中SiO2的衍射峰匹配度极高，说明黑色页岩中含有大量SiO2晶体。
图2为黑色页岩的红外光谱图，从图中可以看出在波数为1 083 cm-1和800 cm-1处出现较强吸收峰，分别为Si-O-Si的伸缩振动峰和硅氧四面体的吸收峰，也与XRD的结论相一致；波数为1 635 cm-1、3 419 cm-1处也出现了吸收峰，为黑色页岩表面或结构中由OH基团伸缩振动产生对称与不对称的吸收峰；波数为3 617 cm-1处出现了结晶水或吸附水的吸收峰；波数为1 422 cm-1附近的吸收峰为羧酸盐的对称伸缩振动吸收峰。
图3为黑色页岩的热失重曲线，从图中可以看出黑色页岩在温度为50～200℃的质量损失率为2.18%，主要为吸附水和结晶水的损失；温度为200～467℃的质量损失率为3.81%，主要为有机碳的裂解；第3段分解实际起始和终止温度为467℃和567℃，质量损失率为5.43%，主要是一些碳酸盐的热分解；温度为750℃后曲线基本平稳，残留率为87.62%。
图4为黑色页岩的XPS谱图，从图中可以看出黑色页岩除含有Si元素和O元素外，还含有C元素、S元素以及Al、Fe金属元素。
图5为黑色页岩的EDS能谱图，从图中可以看出黑色页岩元素组成与XPS数据吻合度较高，还可以看出黑色页岩中还含有少量K、Ca、Ti和Mg等金属元素。以上测试结果说明黑色页岩中含有大量SiO2以及氧化铝、有机碳、微量的硫化亚铁和金属氧化物。通过EDS对黑色页岩的各类元素进行测定，结果表明桂林地区页岩的二氧化硅含量超过51%，黏土约占39%，有机碳约占8%，并含有少量金属氧化物，这与地质研究的结果基本一致[14]。
图6为黑色页岩的SEM图，从图中可以看出页岩粉末为不规则多层片状结构，平均粒径为6.5 μm，片层平均厚度为10.75 nm，体现了黑色页岩为沉积岩的纳米堆叠特征。
2.2 不同偶联剂及表面活性剂对黑色页岩/HDPE复合材料熔融指数的影响
图7为黑色页岩/HDPE复合材料熔融指数与页岩质量份的变化关系。从图7可以看出，随着页岩填充量的增加，黑色页岩/HDPE复合材料的熔融指数均呈现出先升高后下降的趋势，当页岩填充量小于20份时，复合材料的熔融指数随页岩含量的增加逐渐升高，说明HDPE与黑色页岩之间有较好的包裹作用，黑色页岩提升了HDPE的流动性能。当页岩填充量超过20份时，HDPE与黑色页岩开始出现相分离，少量页岩与HDPE之间无牢固的界面粘接，页岩在复合体系中起到阻碍作用，因而复合材料的熔融指数开始出现下降。黑色页岩/HDPE复合材料的熔融指数均为6.5～9.2，没有大幅降低，为黑色页岩/HDPE复合材料的共混挤出以及注塑提供了良好的流动性能，有利于页岩的大量填充。
2.3 不同偶联剂及表面活性剂对黑色页岩/HDPE复合材料拉伸性能的影响
表1为黑色页岩/HDPE复合材料的拉伸强度，纯HDPE的拉伸强度为24.43 MPa。从表1可以看出，5组不同配方的复合材料拉伸强度较纯HDPE均有所下降，每种配方基本都符合拉伸强度随页岩填充量的增加而降低的规律。拉伸强度最高的为KH560+OTAB体系中页岩填充量为5份的复合材料，拉伸强度为24.41 MPa，拉伸强度最低的为ACA+CTAB体系中页岩填充量为50份的复合材料，拉伸强度为22.16 MPa。尽管黑色页岩降低了复合材料的拉伸强度，但页岩填充量达到50份时，黑色页岩/HDPE复合材料的拉伸强度仍超过22 MPa，为页岩的大量填充及降低复合材料的加工成本提供了可能。通过对比表1中偶联剂相同情况下，不同离子表面活性剂对黑色页岩/HDPE复合材料拉伸性能的影响，发现含阴离子表面活性剂配合偶联剂的复合材料拉伸强度均高于含有阳离子表面活性剂配合偶联剂的复合材料。说明相对于阳离子表面活性剂，阴离子表面活性剂能更好地与偶联剂产生协同作用，改善页岩与HDPE的相容性。当页岩填充量为50份时，ACA+SDBS配方的黑色页岩/HDPE复合材料拉伸强度保持最高。与此同时，从含有KH560偶联剂配方中可以看出，烷基链相对较短的阳离子表面活性剂的效果优于烷基链相对较长的阳离子表面活性剂。
2.4 不同偶联剂及表面活性剂对黑色页岩/HDPE复合材料冲击性能的影响
表2为黑色页岩/HDPE复合材料的冲击强度。从表2可以看出，黑色页岩的加入对复合材料的冲击性能有较大的影响，冲击强度均出现下降。其中ACA+SDBS体系的冲击强度保持较好，当页岩填充量为50份时，复合材料的冲击强度为6.39 kJ/m2，说明ACA+SDBS体系可以更好地增加页岩与HDPE之间的相互作用，降低页岩的大量填充对复合材料冲击强度的负面影响。冲击强度结果与拉伸强度变化规律有相似的情况，在偶联剂相同的情况下，含有阴离子表面活性剂的配方冲击强度综合下降幅度低于含阳离子表面活性剂配方的复合材料。
2.5 黑色页岩/HDPE复合材料断面形貌研究
图8为页岩填充量为15份时黑色页岩/HDPE复合材料的断面形貌。
从图8可以看出，5种体系的复合材料中均出现黑色页岩发生破碎和片层剥离现象，页岩片层厚度为80～300 nm。复合材料的断面形貌也说明页岩与HDPE基体之间仍有剥离的现象，HDPE未能与页岩形成“插层复合材料结构”，这也是造成黑色页岩/HDPE复合材料力学性能下降的主要原因。在ACA+SDBS体系中，页岩颗粒脱离HDPE的现象较少，也说明ACA+SDBS体系能够促进页岩与HDPE之间的相互粘接，在提高页岩填充量的情况下，还可以保持复合材料的力学性能。
2.6 不同偶联剂及表面活性剂对黑色页岩/HDPE复合材料热稳定性能的影响
图9为黑色页岩/HDPE复合材料的热重曲线。从图9可以看出，页岩的填充基本不会影响复合材料的初始分解温度，也不会影响复合材料的分解终止温度，说明黑色页岩/HDPE复合材料的热分解主要以HDPE的热分解为主。随着页岩填充量的增加，黑色页岩/HDPE复合材料的残留率逐渐增大，这主要是所填充页岩的热分解产物随填充量增加而增加造成的。当页岩填充量为50份时，ACA+CTAB体系的残留率最大，其值为37.1%，ACA+SDBS体系的残留率最小，其值为21.1%；而偶联剂复配阳离子表面活性剂体系的残留率均大于阴离子体系，主要是由于阴离子促进了偶联剂和页岩之间的相互粘接，在热分解过程中，HDPE也促进了页岩的分解，从而导致黑色页岩/HDPE复合材料体系体现出更小的残留率。
2.7 不同偶联剂及表面活性剂对黑色页岩/HDPE复合材料电性能的影响
表3为不同体系复合材料的体积电阻率测试结果，HDPE的体积电阻率为5.50×1016 Ω·cm。
从表3可以看出，随着页岩填充量的增加，复合材料的体积电阻率逐渐降低，这是因为复合材料的体积电阻主要取决于载流子的迁移率，而载流子的迁移率主要取决于载流子的数量和复合材料中可以束缚载流子的陷阱数量[15]。由于黑色页岩具有导电能力，页岩填充量的增加使得复合材料中载流子数量增多且迁移变得更加容易，同时树脂占比的减少也减少了束缚载流子的陷阱数量，导致出现复合材料体积电阻率随着黑色页岩填充量增加而降低的现象。即使不同体系复合材料的体积电阻率都有不同程度的降低，但仍能维持在1014 Ω·cm以上，复合材料依然具有较好的电绝缘性能。
图10为不同体系复合材料在频率为104～106 Hz条件下的介电常数测试结果。从图10可以看出，随着页岩填充量的增加，复合材料的介电常数逐渐增大，黑色页岩填充量为50份时，介电常数较纯HDPE有所提高，而黑色页岩填充量为5份时，其介电常数会稍低于纯HDPE。HDPE材料为非极性电介质，在交变电场下其介电性能通常不会受到影响，此时影响复合材料介电常数的因素应为黑色页岩填料和HDPE之间的界面相互作用[16]。在复合材料体系中，黑色页岩颗粒的位阻作用会限制HDPE分子链的活动能力和载流子的传输，影响材料在交变电场下的极化作用从而使复合材料的介电常数减小；而当黑色页岩颗粒含量增大时，团聚效应带来的影响会使界面相互作用减小，同时带来更多的偶极基团，增强了极化作用，使复合材料的介电常数增大[16-17]。总体而言，黑色页岩的加入对复合材料的介电常数影响较小，能较好地保持HDPE材料的介电性能。
3 结论
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桂林地区的黑色页岩为片层（厚度为10 nm）沉积而成的沙质页岩，二氧化硅含量达51%，并含有黏土矿物、有机碳以及少量的钾长石等。将黑色页岩与HDPE材料复合制备黑色页岩/HDPE复合材料，页岩的填充降低了复合材料的拉伸强度和冲击强度，但复合材料的拉伸强度仍超过22 MPa，体积电阻率仍能保持在1014 Ω·cm以上，介电性能变化较小，绝缘性能下降较小，且不会明显影响HDPE的熔融流动性能，说明黑色页岩可以作为填料应用到HDPE基绝缘材料中。
基金
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  • 国家自然科学基金资助项目(21864010)
  • 广西自然科学基金资助项目(2018GXNSFAA050030)
  • 广西创新驱动发展专项课题(桂科AA19254010)
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2023年第56卷第11期
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doi: 10.16790/j.cnki.1009-9239.im.2023.11.005
  • 接收时间：2022-11-22
  • 首发时间：2025-11-24
  • 出版时间：2023-11-20
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  • 收稿日期：2022-11-22
  • 修回日期：2023-02-23
基金
国家自然科学基金资助项目(21864010)
广西自然科学基金资助项目(2018GXNSFAA050030)
广西创新驱动发展专项课题(桂科AA19254010)
作者信息
    1桂林理工大学 材料科学与工程学院，广西 桂林 541004
    2桂林鸿程矿山设备制造有限公司， 广西 桂林 541000
    3桂林师范高等专科学校 化学与药学系，广西 桂林 541000

通讯作者:

邓卫星（1981-），男（汉族），安徽淮北人，高级实验师，主要从事高分子复合材料的研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2023.11.005
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2种不同金属材料的力学参数
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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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