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Article(id=1241765088827343591, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241765084528181978, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.07.005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1597334400000, receivedDateStr=2020-08-14, revisedDate=1602172800000, revisedDateStr=2020-10-09, acceptedDate=null, acceptedDateStr=null, onlineDate=1773989468056, onlineDateStr=2026-03-20, pubDate=1626710400000, pubDateStr=2021-07-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773989468056, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773989468056, creator=13701087609, updateTime=1773989468056, updator=13701087609, issue=Issue{id=1241765084528181978, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='7', pageStart='1', pageEnd='120', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773989467027, creator=13701087609, updateTime=1773989590112, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241765600834421400, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241765084528181978, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241765600834421401, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241765084528181978, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=37, endPage=42, ext={EN=ArticleExt(id=1241765091037741814, articleId=1241765088827343591, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Influence of Processing Temperature of Master-batch on Properties of HVDC Cable Insulation, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

In order to research the influence of processing temperature of master-batch on the properties of HVDC cable insulation, three kinds of master-batch were prepared at different processing temperatures, and then the insulating properties of HVDC cable insulation manufactured by the master-batch were studied. Impurity detection was carried out at first, and then the chemical structure of crystal points detected by impurity detection was analyzed by attenuated total reflectance infrared spectroscopy (ATR-IR). At last, the electrical and mechanical properties of three HVDC cable insulation were compared. The results show that there are more crystal points detected in the HVDC cable insulation prepared by the master-batch under an excessive processing temperature, and part crystal points are light yellow. Compared with semitransparent crystal points, there is no strong absorption peaks in the infrared spectra of light yellow crystal points, but the excessive processing temperature has a greater negative effect on the electrical properties of HVDC cable insulation, while has a smaller effect on its mechanical properties.

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为了研究绝缘母料加工温度对高压直流电缆绝缘料性能的影响，选用3种加工温度制备绝缘母料，并对采用3种绝缘母料制备的直流电缆绝缘料性能进行了研究。先开展洁净度检测，再通过全反射红外光谱分析了洁净度检测出的晶点的化学键结构，最后对比了3种直流电缆绝缘料的电气性能和力学性能。结果表明：采用加工温度过高的绝缘母料的直流电缆绝缘料中有更多的晶点，且部分晶点为淡黄色；与半透明的晶点相比，淡黄色晶点的红外光谱上并未出现较强的吸收峰，但过高温对直流电缆绝缘料的电气性能有较大的负面影响，而对力学性能的影响较小。

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曾浩（1988-），男（汉族），江苏南京人，高级工程师，研究方向为直流电缆绝缘料和屏蔽料。

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曾浩（1988-），男（汉族），江苏南京人，高级工程师，研究方向为直流电缆绝缘料和屏蔽料。

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曾浩（1988-），男（汉族），江苏南京人，高级工程师，研究方向为直流电缆绝缘料和屏蔽料。

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直流电缆绝缘料绝缘母料绝缘母料加工温度/℃
Aa140
Bb160
Cc220
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3种直流电缆绝缘料的工艺对比

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直流电缆绝缘料绝缘母料绝缘母料加工温度/℃
Aa140
Bb160
Cc220
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尺寸/μm1 kg样品的晶点数量/个
ABC
50～75000
75～100126
100～175252727
175～2502510
＞250008
总计283451
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3种直流电缆绝缘料的晶点统计数据

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尺寸/μm1 kg样品的晶点数量/个
ABC
50～75000
75～100126
100～175252727
175～2502510
＞250008
总计283451
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测试项目ABC

体积电阻率

/(Ω·m)

30℃2.15×10132.74×10136.09×1012
50℃1.21×10131.06×10131.17×1012
70℃1.86×10122.12×10122.4×1011
90℃4.98×10115.24×10115.71×1010

直流电气强度

/(kV/mm)

30℃394381321
50℃355354265
70℃312307248
90℃297298238
场增强因子(FEF)1.171.171.19
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3种直流电缆绝缘料的电气性能

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测试项目ABC

体积电阻率

/(Ω·m)

30℃2.15×10132.74×10136.09×1012
50℃1.21×10131.06×10131.17×1012
70℃1.86×10122.12×10122.4×1011
90℃4.98×10115.24×10115.71×1010

直流电气强度

/(kV/mm)

30℃394381321
50℃355354265
70℃312307248
90℃297298238
场增强因子(FEF)1.171.171.19
), ArticleFig(id=1245055688985129595, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241765088827343591, language=EN, label=Tab.4, caption=Mechanical properties of three kinds of HVDC cable insulation, figureFileSmall=null, figureFileBig=null, tableContent=
项 目ABC
拉伸性能拉伸强度/MPa22.923.522.2
断裂伸长率/%519520536
热延伸性能负荷下伸长率/%757575
冷却后永久变形率/%000
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项 目ABC
拉伸性能拉伸强度/MPa22.923.522.2
断裂伸长率/%519520536
热延伸性能负荷下伸长率/%757575
冷却后永久变形率/%000
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绝缘母料加工温度对高压直流电缆绝缘料性能的影响研究
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曾浩 1 , 高凯 1 , 王传博 1 , 朱智恩 1 , 吴夕科 1 , 杨黎明 1 , 李栋 1 , 赵维佳 2
绝缘材料 | 材料研究 2021,54(7): 37-42
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绝缘材料 | 材料研究 2021, 54(7): 37-42
绝缘母料加工温度对高压直流电缆绝缘料性能的影响研究
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曾浩1, 高凯1, 王传博1, 朱智恩1, 吴夕科1, 杨黎明1, 李栋1, 赵维佳2
作者信息
  • 1南瑞集团有限公司（国网电力科学研究院有限公司），江苏 南京 211106
  • 2全球能源互联网研究院有限公司 先进输电技术国家重点实验室，北京 102209

    • 曾浩（1988-），男（汉族），江苏南京人，高级工程师，研究方向为直流电缆绝缘料和屏蔽料。

Influence of Processing Temperature of Master-batch on Properties of HVDC Cable Insulation
Hao ZENG1, Kai GAO1, Chuanbo WANG1, Zhien ZHU1, Xike WU1, Liming YANG1, Dong LI1, Weijia ZHAO2
Affiliations
  • 1NARI Group Corporation (State Grid Electric Power Research Institute), Nanjing 211106, China
  • 2State Key Laboratory of Advanced Transmission Technology, Global Energy Interconnection Research Institute Co., Ltd., Beijing 102209, China
出版时间: 2021-07-20 doi: 10.16790/j.cnki.1009-9239.im.2021.07.005
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摘要
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为了研究绝缘母料加工温度对高压直流电缆绝缘料性能的影响，选用3种加工温度制备绝缘母料，并对采用3种绝缘母料制备的直流电缆绝缘料性能进行了研究。先开展洁净度检测，再通过全反射红外光谱分析了洁净度检测出的晶点的化学键结构，最后对比了3种直流电缆绝缘料的电气性能和力学性能。结果表明：采用加工温度过高的绝缘母料的直流电缆绝缘料中有更多的晶点，且部分晶点为淡黄色；与半透明的晶点相比，淡黄色晶点的红外光谱上并未出现较强的吸收峰，但过高温对直流电缆绝缘料的电气性能有较大的负面影响，而对力学性能的影响较小。

绝缘母料  /  高压直流电缆  /  洁净度  /  晶点  /  全反射红外光谱  /  电气性能

In order to research the influence of processing temperature of master-batch on the properties of HVDC cable insulation, three kinds of master-batch were prepared at different processing temperatures, and then the insulating properties of HVDC cable insulation manufactured by the master-batch were studied. Impurity detection was carried out at first, and then the chemical structure of crystal points detected by impurity detection was analyzed by attenuated total reflectance infrared spectroscopy (ATR-IR). At last, the electrical and mechanical properties of three HVDC cable insulation were compared. The results show that there are more crystal points detected in the HVDC cable insulation prepared by the master-batch under an excessive processing temperature, and part crystal points are light yellow. Compared with semitransparent crystal points, there is no strong absorption peaks in the infrared spectra of light yellow crystal points, but the excessive processing temperature has a greater negative effect on the electrical properties of HVDC cable insulation, while has a smaller effect on its mechanical properties.

master-batch  /  HVDC cable insulation  /  cleanliness  /  crystal points  /  attenuated total reflectance infrared spectroscopy (ATR-IR)  /  electrical properties
曾浩, 高凯, 王传博, 朱智恩, 吴夕科, 杨黎明, 李栋, 赵维佳. 绝缘母料加工温度对高压直流电缆绝缘料性能的影响研究. 绝缘材料, 2021 , 54 (7) : 37 -42 . DOI: 10.16790/j.cnki.1009-9239.im.2021.07.005
Hao ZENG, Kai GAO, Chuanbo WANG, Zhien ZHU, Xike WU, Liming YANG, Dong LI, Weijia ZHAO. Influence of Processing Temperature of Master-batch on Properties of HVDC Cable Insulation[J]. Insulating Materials, 2021 , 54 (7) : 37 -42 . DOI: 10.16790/j.cnki.1009-9239.im.2021.07.005
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0 引言
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随着输送容量需求的不断提高以及跨海工程、洲际联网工程的日益增加，直流输电在电力系统的应用越来越广泛。与交流输电相比，直流输电具有传输容量大、损耗小（基本上只有电阻损耗，没有电磁损耗和介电损耗）、不存在无功功率、电源连接方便、易于调节和控制等优点。同时，直流输电线路没有电容电流的干扰，可靠性更高[1-2]。
作为直流输电的重要装备，交联聚乙烯（XLPE）绝缘电缆在远海风电进网、岛屿供电等领域得到广泛应用。然而，在高压直流作用下，XLPE内部极易积累空间电荷，导致局部电场发生畸变，从而使XLPE内部最大电场比平均电场高出5～11倍[3]，严重情况下甚至会导致绝缘电击穿。国内外的专家针对如何抑制XLPE中的空间电荷方面做了大量的研究，并取得一定成效。一般来说，研究人员采用纳米复合和化学接枝这两种方法抑制XLPE内部的空间电荷[4-9]。由于化学接枝是在乙烯单体合成低密度聚乙烯（LDPE）基料过程中发生的，反应控制难度大、转化率低，而国内电缆绝缘料用LDPE均出自中石化的大设备生产，通过化学接枝的方法很难实现大规模的批量化生产，因此国内科研院所大多采用纳米复合的方法制备高压直流电缆绝缘料。
纳米粒子堆积密度小，添加非常困难，需要先制备绝缘母料，再制备直流电缆绝缘料。绝缘母料是把纳米粒子以超常量（≥10%）添加到LDPE基料中制备的浓缩体。生产直流电缆绝缘料时，不必再添加纳米粒子，只需要添加一定比例的LDPE基料和绝缘母料[10]。
制备绝缘母料时，为了提高纳米粒子在基料中的分散和分布，应尽量提高加工温度，但过高的加工温度会使材料发生热氧老化，甚至会导致材料发生热降解。本文选用3种加工温度制备绝缘母料，先开展洁净度检测，再通过全反射红外光谱分析洁净度检测出的晶点的化学键结构，最后研究3种直流电缆绝缘料的电气性能和力学性能，分析绝缘母料过温加工对直流电缆绝缘料性能的影响。
1 试验
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1.1 主要原材料
基料为扬子—巴斯夫公司生产的LDPE，密度约为0.92 g/cm3，熔体流动速率为2.0 g/10 min；空间电荷抑制剂为一种高比表面积无机纳米粒子，比表面积为100～150 m2/g；助剂为进口抗氧剂300，密度为1.1 g/cm3，灰分含量≤0.05%。
1.2 试样制备
采用失重秤分别将基料和质量分数为0.4%的助剂通过主喂料口加入双螺杆挤出机，将质量分数为10%的纳米粒子通过侧喂料机输送至双螺杆挤出机，绝缘母料制备流程如图1所示，将不同加工温度（挤出机各段的最高加热温度）的绝缘母料分别记为a、b、c。分别将3种绝缘母料通过往复式单螺杆挤出机按照一定比例稀释，经500目滤网过滤，水下切粒后采用后渗透法添加一定比例交联剂，制备成直流电缆绝缘料，其流程图如图2所示，将采用不同绝缘母料制备的直流电缆绝缘料分别记为A、B、C，具体如表1所示。
1.3 测试方法
1.3.1 洁净度（OCS）检测
按照JB/T 10437—2004规定通过OCS高精度光学系统，检测1 kg流涎膜样品中杂质与晶点的数量与尺寸，流延膜厚度为0.1 mm。
1.3.2 全反射红外光谱分析
采用Thermo Fisher Scientific公司的Nicolet is10型红外光谱仪进行测试，配备Smart iTX衰减全反射附件，扫描次数32次，扫描范围为4 000～525 cm-1。
1.3.3 体积电阻率测试
按照GB/T 1410—2006规定进行测试，试片厚度为1.0 mm，每组至少5个样品，试验温度分别为30、50、70、90℃。考虑到实际工程中直流电缆绝缘层的平均场强为10～20 kV/mm，因此体积电阻率测试采用20 kV作为测试电压。为了改善金属电极与试片的接触，试片表面涂覆导电银漆作为电极材料。
1.3.4 直流电气强度测试
按照GB/T 1408—2006规定进行测试，试片厚度为0.3 mm，每组至少10个样品，周围媒介为绝缘油，电极为球形电极，试验温度分别为30、50、70、90℃。试验采用快速升压方式，升压速度为5 kV/s。
1.3.5 空间电荷测试
采用压力波法（PWP法）[11-12]开展空间电荷测试，PWP法空间电荷测试系统如图3所示。绝缘样品的两面需热贴半导电层，其中绝缘层厚度为 1 mm，直径为170 mm，半导电层厚度为0.5 mm，直径为50 mm。测试温度为40℃，对试样施加-40 kV直流电压（平均场强为40 kV/mm），保持60 min，记录60 min时的空间电荷分布波形。
1.3.6 拉伸性能测试
按照GB/T 1040—2006规定进行测试，试片为2型哑铃片，厚度为1.0 mm，每组至少5个样品，标距长度为25 mm，拉伸速度为250 mm/min。
1.3.7 热延伸性能测试
按照GB/T 2951.21—2008规定进行测试，试片为GB/T 1040—2006规定的2型哑铃片，厚度为1.0 mm，负重为0.2 MPa，每组至少3个样品。
2 结果与分析
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2.1 洁净度检测
在高压电场下，任何能引起电缆绝缘层局部电场畸变的物质，都可能给绝缘带来危害。虽然直流电气强度在一定程度上能够反映绝缘料的耐压性能，但对整根电缆来说，绝缘料中任意一处的杂质也可能造成电缆的击穿[13]，因此，评估高压电缆绝缘料时OCS检测是必不可少的。
通过检测发现，3种直流电缆绝缘料均无尺寸大于50 μm的黑点，但存在一定数量的晶点，具体晶点统计如表2所示。
晶点是聚乙烯薄膜制品中常见的缺陷，可能是聚乙烯中熔点较高的部分，也有可能是由于加工温度过高聚乙烯发生了热氧老化，甚至热降解。从表2可以看出，3种直流电缆绝缘料均存在不同尺寸的晶点，其中直流电缆绝缘料C的晶点数量明显高于直流电缆绝缘料A和B，甚至存在尺寸大于250 μm的晶点。
剪下OCS检测出较大尺寸晶点的薄膜，在显微镜下观察晶点的颜色。图4和图5分别为A、B、C样品薄膜上OCS检测出的晶点典型图。
从图4和图5可以看出，直流电缆绝缘料A和B的晶点为半透明状物质，而直流电缆绝缘料C中存在部分淡黄色晶点，可能是因为绝缘母料制备过程中加工温度过高产生的，具体成分需通过全反射红外光谱分析。
2.2 全反射红外光谱分析
聚合物材料的热氧老化是按照链式自由基机理进行的具有自动催化特征的氧化反应，其过程由链引发、链增长、链终止3个阶段组成。
①链引发：聚合物分子链受热分解形成自由基，如式（1）所示。
RH→R·+H·
②链增长：遇到空气后，活性的烷基自由基（R·）与氧分子结合生成过氧自由基（ROO·），ROO·能够夺取聚合物分子链上的H，从而生成过氧化氢（ROOH）和新的R·，而ROOH不稳定，受热分解成含羰基（C=O）的自由基（RO·）和羟基（·OH），如式（2）～（4）所示。
R·+O2→ROO·
ROO·+RH→ROOH+R·
ROOH→RO·+·OH
③链终止：自由基之间相互结合形成惰性物质，从而使链终止，如式（5）～（6）所示。
R·+R·→R-R
RO·+R·→ROR
聚合物热氧老化的标志性化学结构变化是 C=O的生成，C=O吸收峰在红外光谱上最为明显。图6是4种试样的红外光谱图，其中基料为未进行二次加工的LDPE试样，直流电缆绝缘料A、B、C为3种含晶点的试样，老化料为直流电缆绝缘料C在135℃下老化处理168 h的试样。
由图6可以看出，基料的红外光谱是典型的LDPE红外吸收峰，在约2 950、1 460、720 cm-1处有3个强烈的吸收峰，分别代表C-H的伸缩、弯曲和摇摆特征峰。与基料相比，直流电缆绝缘料A、B、C晶点的红外光谱在1 725～1 600 cm-1和1 300～1 100 cm-1处存在较弱的吸收峰，而老化料的红外光谱在相同位置上的吸收峰较强烈，特别是1 725 cm-1处的老化特征峰（C=O）、1 600 cm-1处的断链特征峰（H2C=CR1R2或R1CH=CR2R3），以及1 250 cm-1处的C-O特征峰。
此外，3种直流料的晶点和老化料在3 800～3 600 cm-1处存在较弱的吸收峰，该区域为-OH的特征吸收区域，应该是加工之后样品中的水分导致。
2.3 电气性能
与交流电缆绝缘料需要考察四大电气参数不一样，一般可以通过体积电阻率/电导率、直流电气强度、空间电荷性能来评价直流电缆绝缘料的电气性能[14]，表3是3种直流电缆绝缘料的电气性能对比。从表3可以看出，在不同测试温度下，直流电缆绝缘料A和直流电缆绝缘料B的体积电阻率和直流电气强度非常接近，而直流电缆绝缘料C的大部分测试数据则与两者相差较多。
直流电场是根据电阻率分布的，而对于所有绝缘材料，电阻率均随温度上升而呈指数下降，一般可用式（7）表示。
ρ=ρ0⋅e-aθ
式（7）中：ρ0为温度为0℃时的电阻率；ρ为温度为θ时的电阻率；a为电阻率温度系数，反映电阻率随温度变化的敏感程度。
根据表3中的数据计算得到直流电缆绝缘料A、B和C的电阻率温度系数分别为0.066、0.067和0.078，较低的电阻率温度系数表明直流电缆绝缘料的电阻率随温度变化较小，直流电缆运行时，绝缘层电场分布更加均匀。
通过场增强因子FEF（field enhancement factor）[15-16]可以表征空间电荷注入情况，如式（8）所示。
FEF=νpeakνpeak,cal·UcalU
式（8）中：νpeak为施加40 kV高压时的地电极信号电压，单位为mV；νpeak,cal为在无空间电荷注入时低电压Ucal下的校准地电极信号电压，单位为mV。
FEF的值越大，表示空间电荷注入越多，从表3可以看出，直流电缆绝缘料C的空间电荷抑制效果稍差于直流电缆绝缘料A和B。
2.4 力学性能
除了电气性能外，力学性能也是直流料开发需要考虑的因素。表4是3种直流电缆绝缘料的拉伸性能和热延伸性能测试数据。由表4可以看出，3种直流电缆绝缘料的力学性能非常接近。与直流电缆绝缘料A和B中半透明的晶点相比，直流电缆绝缘料C中淡黄色晶点的红外光谱上并未出现较强的吸收峰，对直流电缆绝缘料的力学性能影响较小。
3 讨论
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从洁净度OCS的检测结果来看，采用加工温度过高的绝缘母料c的直流电缆绝缘料C中检测出更多的晶点，且存在部分淡黄色晶点。通过全反射红外光谱分析发现，与基料相比，3种直流电缆绝缘料均发生了热氧老化，但热氧老化的程度较浅，没有明显的C=O生成。与半透明的晶点相比，淡黄色晶点的红外光谱上并未出现较强的吸收峰，可能是因为绝缘母料的加工时间还不够长，更长时间的加工会增加材料的热氧老化程度，从而产生深黄色甚至褐色的晶点。
从3种直流电缆绝缘料的电气性能和力学性能测试结果来看，直流电缆绝缘料A和直流电缆绝缘料B的电气性能相当，而直流电缆绝缘料C的电气性能整体劣于前两者，3种直流电缆绝缘料的力学性能非常接近。虽然淡黄色晶点的化学键结构没有检测出明显变化，但在高电场下，这些晶点可能会发生电离形成载流子，可自由移动的载流子数量的增加会导致直流电缆绝缘料的体积电阻率下降；同时晶点电离还可能形成异极性电荷[17]，异极性空间电荷的不断积聚会导致绝缘内部电场的局部畸变，不仅会增大FEF的数值，还会间接影响绝缘料的直流电气强度。因此，在长时间、批量化制备绝缘母料时，严格控制加工温度至关重要。
4 结论
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（1）相比于直流电缆绝缘料A和B，采用加工温度过高的绝缘母料c的直流电缆绝缘料C中有更多的晶点，其中直流电缆绝缘料A和B的晶点为半透明色，而直流电缆绝缘料C中的晶点为淡黄色。
（2）与基料相比，3种直流电缆绝缘料均发生了热氧老化，但热氧老化的程度较浅，没有明显的C=O生成。与半透明的晶点相比，淡黄色晶点的红外光谱上并未出现较强的吸收峰。
（3）绝缘母料加工温度过高对直流电缆绝缘料的电气性能有较大的负面影响，但对力学性能的影响较小。
基金
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  • 国家电网有限公司总部科技项目(5500-201958320A-0-0-00)
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doi: 10.16790/j.cnki.1009-9239.im.2021.07.005
  • 接收时间：2020-08-14
  • 首发时间：2026-03-20
  • 出版时间：2021-07-20
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  • 收稿日期：2020-08-14
  • 修回日期：2020-10-09
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国家电网有限公司总部科技项目(5500-201958320A-0-0-00)
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    1南瑞集团有限公司（国网电力科学研究院有限公司），江苏 南京 211106
    2全球能源互联网研究院有限公司 先进输电技术国家重点实验室，北京 102209
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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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