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Article(id=1210577667628340112, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210577662121209865, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.08.005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1683993600000, receivedDateStr=2023-05-14, revisedDate=1713715200000, revisedDateStr=2024-04-22, acceptedDate=null, acceptedDateStr=null, onlineDate=1766553807407, onlineDateStr=2025-12-24, pubDate=1724083200000, pubDateStr=2024-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766553807407, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766553807407, creator=13701087609, updateTime=1766553807407, updator=13701087609, issue=Issue{id=1210577662121209865, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='8', pageStart='1', pageEnd='147', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766553806095, creator=13701087609, updateTime=1766563971278, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210620298043454173, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210577662121209865, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210620298043454174, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210577662121209865, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=46, endPage=51, ext={EN=ArticleExt(id=1210577667942912929, articleId=1210577667628340112, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Relationship between comprehensive properties of low dielectric ink containing multi-fluorinated poly(aryl ether) and active diluents, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

With the rapid development in the field of microelectronics and microelectronics processing technology, manufacturing microelectronic devices using inkjet printing technology has become a popular direction in additive manufacturing. In this paper, an UV-curable vinyl-terminated polyarylether prepolymer was prepared by nucleophilic substitution reaction with twisted non-coplanar phthalazinone and hexafluoroisopropyl as structural units. A new low dielectric ink system for 3D printing was constructed by using diacrylate reactive diluents and free radical fast initiators into the prepolymer. The results show that the viscosity of the ink system before curing is lower than 300 mPa·s,indicating good processability. After UV and thermal curing, the infrared testing shows that the curing degree can reach over 87%, and the curing is basically complete. The minimum volume shrinkage is only 2.4%, which indicate the ink has excellent dimensional stability. The glass transition temperature of the material can reach up to 210℃, and the thermal decomposition temperature can reach up to 370℃, which indicate the ink has the potential of long-term use at 150℃. At 10 GHz, the dielectric constant of the material can reach 2.61, and the dielectric loss factor is only 0.014, which indicate the ink has excellent dielectric properties. The ink system prepared in this study is applicable to the additive manufacturing process of large curvature conformal circuit and has good application prospect in the field of microelectronics.

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随着微电子领域和微电子加工技术的快速发展，通过喷墨打印技术制造微电子器件已经成为当前热门的增材制造方向。本文以扭曲非共平面的杂萘联苯和六氟异丙基为结构基元，通过亲核取代反应制备了可紫外光固化的乙烯基封端的聚芳醚预聚物，加以不同种类的双丙烯酸酯类活性稀释剂和自由基类快速光引发剂共同构建新型3D打印低介电油墨体系。结果表明：油墨体系固化前的黏度均低于300 mPa·s，可加工性能良好；经UV和热固化后，红外测试表明其固化程度可达87%以上，固化基本完全；体积收缩率最低仅为2.4%，具有优异的尺寸稳定性；材料的玻璃化转变温度最高可达210℃，热分解温度最高达370℃，具备在150℃下长期使用的潜力；在10 GHz测试频率下材料介电常数可达2.61，介质损耗因数仅为0.014，具有优异的介电性能。本研究制备的油墨体系可适用大曲率共形电路增材制造工艺，在微电子领域具有良好的应用前景。

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苑博（1987-），男（汉族），四川成都人，高级工程师，主要从事射频天线设计与制造、材料加工与应用、绝缘材料制备与性能调控的研究。

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苑博（1987-），男（汉族），四川成都人，高级工程师，主要从事射频天线设计与制造、材料加工与应用、绝缘材料制备与性能调控的研究。

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苑博（1987-），男（汉族），四川成都人，高级工程师，主要从事射频天线设计与制造、材料加工与应用、绝缘材料制备与性能调控的研究。

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活性稀释剂油墨黏度/(mPa·s)
EDG111.6
HD116.2
TGD285.4
NGD112.5
DGD85.0
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不同UV固化体系黏度

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活性稀释剂油墨黏度/(mPa·s)
EDG111.6
HD116.2
TGD285.4
NGD112.5
DGD85.0
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体系UV固化程度/%热固化程度/%
PEDG90765.4169.17
PEDG18450.2055.52
PHD90761.7064.53
PHD18469.4778.95
PTGD90769.6476.81
PTGD18477.6078.42
PNGD90779.9083.68
PNGD18483.0886.12
PDGD90775.6687.37
PDGD18470.3271.82
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不同UV固化油墨体系的转化率

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体系UV固化程度/%热固化程度/%
PEDG90765.4169.17
PEDG18450.2055.52
PHD90761.7064.53
PHD18469.4778.95
PTGD90769.6476.81
PTGD18477.6078.42
PNGD90779.9083.68
PNGD18483.0886.12
PDGD90775.6687.37
PDGD18470.3271.82
), ArticleFig(id=1218111681083921226, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577667628340112, language=EN, label=Table 3, caption=Thermal properties of different UV ink systems after curing, figureFileSmall=null, figureFileBig=null, tableContent=
体系Tg/℃Td5%/℃
PEDG907149270
PEDG184155270
PHD907135370
PHD184145371
PTGD907210320
PTGD184195320
PNGD907124350
PNGD184129330
PDGD907182334
PDGD184190335
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不同UV油墨体系固化后的热性能

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体系Tg/℃Td5%/℃
PEDG907149270
PEDG184155270
PHD907135370
PHD184145371
PTGD907210320
PTGD184195320
PNGD907124350
PNGD184129330
PDGD907182334
PDGD184190335
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体系紫外线固化收缩率/%紫外线+热固化收缩/%
PEDG1843.25.0
PHD1842.73.6
PTGD1841.72.4
PNGD1845.06.2
PDGD1842.83.5
), ArticleFig(id=1218111681360745309, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577667628340112, language=CN, label=表4, caption=

不同UV油墨体系固化后的固化收缩率

, figureFileSmall=null, figureFileBig=null, tableContent=
体系紫外线固化收缩率/%紫外线+热固化收缩/%
PEDG1843.25.0
PHD1842.73.6
PTGD1841.72.4
PNGD1845.06.2
PDGD1842.83.5
), ArticleFig(id=1218111681469797222, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577667628340112, language=EN, label=Table 5, caption=Mechanical properties of different UV cured resin films, figureFileSmall=null, figureFileBig=null, tableContent=
薄膜弹性模量/MPa抗拉强度/MPa断裂伸长率/%
PHD1842123.42.3
PTGD18499310.91.6
PNGD1841161.18.4
PDGD1844132.73.8
), ArticleFig(id=1218111681557877611, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577667628340112, language=CN, label=表5, caption=

不同UV固化树脂薄膜的力学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
薄膜弹性模量/MPa抗拉强度/MPa断裂伸长率/%
PHD1842123.42.3
PTGD18499310.91.6
PNGD1841161.18.4
PDGD1844132.73.8
), ArticleFig(id=1218111681683706740, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577667628340112, language=EN, label=Table 6, caption=Dielectric properties of different UV cured resin films, figureFileSmall=null, figureFileBig=null, tableContent=
薄膜Dk,10GHzDf,10GHzDk,28GHzDf,28GHz
PEDG1842.880.0312.880.029
PHD1843.030.0223.080.022
PTGD1842.610.0142.820.015
PNGD1842.960.0193.240.019
), ArticleFig(id=1218111681788564350, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577667628340112, language=CN, label=表6, caption=

不同UV固化树脂薄膜的介电性能

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薄膜Dk,10GHzDf,10GHzDk,28GHzDf,28GHz
PEDG1842.880.0312.880.029
PHD1843.030.0223.080.022
PTGD1842.610.0142.820.015
PNGD1842.960.0193.240.019
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活性稀释剂与多氟聚芳醚低介电油墨综合性能关系研究
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苑博
绝缘材料 | 材料研究 2024,57(8): 46-51
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绝缘材料 | 材料研究 2024, 57(8): 46-51
活性稀释剂与多氟聚芳醚低介电油墨综合性能关系研究
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苑博
作者信息
  • 中国电子科技集团公司第十研究所，四川 成都 610036

    • 苑博（1987-），男（汉族），四川成都人，高级工程师，主要从事射频天线设计与制造、材料加工与应用、绝缘材料制备与性能调控的研究。

Relationship between comprehensive properties of low dielectric ink containing multi-fluorinated poly(aryl ether) and active diluents
Bo YUAN
Affiliations
  • The tenth Research Institute of China Electronics Technology Group Corporation, Chengdu 610036, China
出版时间: 2024-08-20 doi: 10.16790/j.cnki.1009-9239.im.2024.08.005
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摘要
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随着微电子领域和微电子加工技术的快速发展，通过喷墨打印技术制造微电子器件已经成为当前热门的增材制造方向。本文以扭曲非共平面的杂萘联苯和六氟异丙基为结构基元，通过亲核取代反应制备了可紫外光固化的乙烯基封端的聚芳醚预聚物，加以不同种类的双丙烯酸酯类活性稀释剂和自由基类快速光引发剂共同构建新型3D打印低介电油墨体系。结果表明：油墨体系固化前的黏度均低于300 mPa·s，可加工性能良好；经UV和热固化后，红外测试表明其固化程度可达87%以上，固化基本完全；体积收缩率最低仅为2.4%，具有优异的尺寸稳定性；材料的玻璃化转变温度最高可达210℃，热分解温度最高达370℃，具备在150℃下长期使用的潜力；在10 GHz测试频率下材料介电常数可达2.61，介质损耗因数仅为0.014，具有优异的介电性能。本研究制备的油墨体系可适用大曲率共形电路增材制造工艺，在微电子领域具有良好的应用前景。

紫外固化  /  喷墨打印  /  低介电常数  /  杂萘联苯  /  聚芳醚

With the rapid development in the field of microelectronics and microelectronics processing technology, manufacturing microelectronic devices using inkjet printing technology has become a popular direction in additive manufacturing. In this paper, an UV-curable vinyl-terminated polyarylether prepolymer was prepared by nucleophilic substitution reaction with twisted non-coplanar phthalazinone and hexafluoroisopropyl as structural units. A new low dielectric ink system for 3D printing was constructed by using diacrylate reactive diluents and free radical fast initiators into the prepolymer. The results show that the viscosity of the ink system before curing is lower than 300 mPa·s,indicating good processability. After UV and thermal curing, the infrared testing shows that the curing degree can reach over 87%, and the curing is basically complete. The minimum volume shrinkage is only 2.4%, which indicate the ink has excellent dimensional stability. The glass transition temperature of the material can reach up to 210℃, and the thermal decomposition temperature can reach up to 370℃, which indicate the ink has the potential of long-term use at 150℃. At 10 GHz, the dielectric constant of the material can reach 2.61, and the dielectric loss factor is only 0.014, which indicate the ink has excellent dielectric properties. The ink system prepared in this study is applicable to the additive manufacturing process of large curvature conformal circuit and has good application prospect in the field of microelectronics.

UV curing  /  3D printing  /  low dielectric constant  /  phthalazinone  /  polyarylether
苑博. 活性稀释剂与多氟聚芳醚低介电油墨综合性能关系研究. 绝缘材料, 2024 , 57 (8) : 46 -51 . DOI: 10.16790/j.cnki.1009-9239.im.2024.08.005
Bo YUAN. Relationship between comprehensive properties of low dielectric ink containing multi-fluorinated poly(aryl ether) and active diluents[J]. Insulating Materials, 2024 , 57 (8) : 46 -51 . DOI: 10.16790/j.cnki.1009-9239.im.2024.08.005
正文
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0 引言
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3D打印属于新型增材制造技术，与传统减材制造方法不同，该方法通过电脑生成的打印模型数据，采用增材逐层打印来制造产品。3D打印技术最开始是由美国的3M公司和UVP公司在20世纪80年代提出并推广，发展至今，3D打印技术在制造业领域已经取得了较为广泛的应用[1-2]。
3D打印技术目前可分为熔融沉积（FDM）技术[3-4]、光固化（SLA）技术[5-6]、选择性激光烧结（SLS）技术[7-8]、叠层实体（LOM）技术[9-10]和聚合物喷射（PolyJet）打印技术[11]等。其中聚合物喷射打印技术主要是通过将液态的光敏树脂喷射到平台上，并控制喷射液体的用量使其具有一定形状，然后用紫外光照射，等待固化完全后再喷射第二层树脂，并再次光固化，如此循环往复，逐层打印材料。PolyJet打印技术是由美国的Stratasys公司首次提出。其油墨一般由三部分组成，包括光引发剂、预聚物以及活性稀释剂等。根据实际需求，可少量添加相关助剂，以满足材料具体的应用需求[12]。以上3种主要成分中，预聚物是PolyJet油墨中的最重要组分，决定了树脂打印成型后的主要性能。目前3D打印油墨所采用的预聚物以多官能度不饱和树脂为主，这类树脂耐热性低、机械强度低、介电常数大，限制了PolyJet技术在低介电结构材料领域中的应用。
聚芳醚具有高强度、低介电、耐酸碱腐蚀性良好、热性能优异和吸湿性低等特点。然而，由于其缺少可紫外光（UV）固化的交联点，无法作为预聚物应用于3D打印增材制造领域。因此，为了引入低介电、高强度的聚芳醚作为预聚物改性3D油墨的综合性能，本文合成了以烯烃为端基的杂萘联苯聚芳醚，选取双官能团丙烯酸酯作为活性稀释剂，并加入高效光引发剂，配制低介电UV光固化油墨，构建新型3D打印低介电油墨体系。为了提升预聚物在活性稀释剂中的溶解度和添加量，引入非扭曲共平面的杂萘联苯结构。利用该结构的大体积和芳香性，在提升聚芳醚溶解性的同时，改善3D打印树脂的力学性能和介电性能。
1 实验
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1.1 原材料
4-(4-羟基苯基)-2,3-二氮杂萘-1-酮（DHPZ），自制；双酚AF（6F-BPA），西陇化学厂；十氟联苯（DFBP），天津化学试剂二厂；五氟苯乙烯（FSt），Sigma-Aldrich公司。活性稀释剂分为5种：乙二醇二甲基丙烯酸甲酯（EDG）、二丙烯酸1，6-己二醇酯（HD）、二缩三丙二醇二丙烯酸酯（TGD）、新戊二醇二丙烯酸酯（NGD）、二丙二醇二丙烯酸酯（DGD），均购自上海麦克林生化科技有限公司。光引发剂分为1-羟基环己基苯酮（184）、（2-甲基-2-(4-吗啉基)-1-[4-(甲硫基)苯基]-1-丙酮（907），均购自上海毕得医药科技有限公司。其他常用试剂溶剂：三乙醇胺、N,N-二甲基乙酰胺（DMAc）、碳酸钾、无水乙醇、甲苯、浓盐酸等，均购自博迪化工有限公司。
由于活性稀释剂均含有阻聚剂，在进行UV固化油墨时需先将单体中的阻聚剂除去，否则会影响UV固化性能。方法如下：取少量待处理单体与少量质量分数为5%的NaOH溶液混合，置于分液漏斗中（单体与NaOH溶液的体积比为1∶1.5），反复振荡，静置分层，该过程重复3次。随后从分液漏斗收集油相，并加入少量无水硫酸镁吸收油相中残余的水分，静置30 min后进行过滤，并收集滤液。最后经过减压蒸馏后得到高纯度活性稀释剂。其余试剂均在购买后直接使用。
1.2 制备过程
1.2.1 五氟苯乙烯基封端聚芳醚的合成
五氟苯乙烯基封端聚芳醚（FSt-FPPE）预聚物的合成路线方程式如图1所示。
在装有机械搅拌、分水器和氮气导管的100 mL三口烧瓶中加入11 mmol的 DHPZ、7 mmol的 6F-BPA、25 mmol碳酸钾和30 mL甲苯，在通入氮气后于130℃下甲苯冷却回流2 h。随后将甲苯完全蒸出后冷却至110℃，加入2 mmol五氟苯乙烯和少量DMAc（约3 mL），在110℃条件下避光反应1 h。然后加入17 mmol 的DFBP和5 mL N,N-二甲基乙酰胺溶剂，继续避光反应5 h，若体系中途变黏稠则补加少许溶剂防止产物交联。直至体系黏度不再增加后（中心液面不再升高）停止反应。然后将产物沉降过滤，反复煮沸5次后，用80℃烘箱烘干24 h，得到聚合物初产物。最后配制0.1 g/ml的DMAc溶液溶解聚合物初产物，用硅藻土过滤，除去不溶杂质与残留的金属离子，并沉降于乙醇溶液中，最后得到白色絮状物沉淀预聚物，计算收率为83%。通过凝胶渗透色谱法（GPC）检测，预聚物数均分子量（Mn）为9 100，重均分子量（Mw）为16 400，分子量分布（PD）为1.8。预聚物核磁谱图及其各质子峰归属如图2所示，从图2可以看出，所有峰均得到较好归属，表明合成的预聚物FSt-FPPE结构与设计一致。
1.2.2 喷墨打印介电油墨的配制
3D打印的油墨配方为：活性单体质量分数为75%，预聚物FSt-FPPE质量分数为20%，光引发剂质量分数为5%，活性稀释剂和光引发剂的结构与缩写如图3所示。取一定质量FSt-FPPE加入在相应质量比的活性稀释剂单体中，然后将混合物放入玻璃瓶，置于磁力搅拌器上搅拌以促进FSt-FPPE的溶解，若瓶中有不溶物则置于超声波溶解仪中，通过超声波振荡促进溶解，样品制成后用铝箔纸包裹，在低温、避光的条件下储存。
1.2.3 UV固化过程以及热固化过程
采用OPAS XLite 600 UV型烘箱进行紫外固化，UV主峰波长为365 nm，输出功率为1 000 W，紫外固化时间为30 s。将固化油墨浇注于玻璃平板上，并用另一块玻璃板放置于垫片上方，防止氧阻聚现象发生。再将紫外固化后的样品放置于120℃烘箱中，热固化30 min。
1.2.4 UV固化薄膜的制备
将UV固化油墨浇注于玻璃板，均匀刮涂成厚度为0.25 mm的薄膜，紫外固化30 s，并于120℃下固化30 min，待固化完全后，裁成固定尺寸，用于介电性能测试和拉伸强度测试。样品的命名以PEDG184为例，P代表固化后的聚合物树脂；EDG表示活性稀释剂种类，184代表光引发剂种类，以此类推。UV固化体系各材料简称详见1.1节。
1.3 测试与表征
红外光谱测试使用Thermo Nicolet IS50型高级傅里叶变换红外光谱仪（FTIR），固化程度通过红外谱图中双键峰的强度判断，选择反应前后无变化的羰基峰作为参比，采用反射法进行测试，观测波数范围为500～4 000 cm-1。核磁测试使用布鲁克公司的Bruker AVANCE Ⅲ 5000型核磁共振波谱仪，采用氘代氯仿为溶剂，使用四甲基硅烷作为化学位移内标，测试温度为25℃。凝胶渗透色谱分析采用 HP1090型高效液相色谱仪，以NMP作为溶剂，并串联5 mm色谱柱，采用阴离子聚合聚苯乙烯作为标准样品。聚合物的热转变测试使用TA Q20型差示扫描量热仪，氮气流量为50 mL/min，升温速率为10℃/min，玻璃化转变温度（Tg）取值为扫描曲线上热熔变化的中点，扫描温度范围为30～450℃。聚合物的热失重测试使用TA Q500型热重仪，氮气气氛流速为50 mL/min，升温速率为10℃/min，扫描温度范围为30～800℃。力学性能测试使用Instron-5869型拉伸试验机，载荷为500 N，应变速率为 5 mm/min，试样的有效拉伸长度为20 mm，宽度为 6 mm。油墨的黏度测试使用上海尼润智能科技有限公司生产的NTV-E1型数字式旋转黏度计。固化收缩率采用紫外固化和热固化前后样品的尺寸变化计算而得。采用 Agilent E5061A型网络分析仪分别测试聚合物薄膜在10 GHz和28 GHz下的介电常数和介质损耗因数，测试前将聚合物样品置于105 ℃的真空烘箱中烘干2 h，再置于相对湿度为50%、温度为25℃的恒湿箱中静置24 h。
2 结果与讨论
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2.1 UV固化油墨的黏度
配置后的固化油墨黏度如表1所示。UV固化油墨黏度主要受单体分子量与单体黏度的影响，DGD单体黏度最小，因其结构中醚键含量较多，分子链柔性大。TGD单体结构中亦含醚键，但分子量相对较高，且分子链内没有支链，所有结构均在分子链的主链上，使得分子链的运动受到限制，导致其混合后在所有配方中黏度最高。其他3种配方的黏度相差不大，均具有良好的流动性。所有油墨体系均具有较低的黏度，可以适用直写（DIW）和喷墨打印（PolyJet）等增材制造工艺。
2.2 UV固化油墨固化程度
通过红外谱图的碳碳双键特征峰强度，定量分析双键含量，选择单体中不参与反应的羰基峰强度作为参比进行归一化处理，PEDG184固化前后的FTIR谱图如图4所示。从图4可以看出，碳基的吸收峰固化前后强度不变，而C=C双键的吸收峰随着UV固化和热固化有所降低，将该信号进行归一化处理并总结于表2中。
10种油墨配方的具体UV固化程度（转化率）与热固化转化率如表2所示。从表2可以看出，NGD单体的转化率较高，这与NGD本身结构有关，其主链长度最短，同时分子量低，因此黏度小，油墨混合比较均匀。同时此配方的双键浓度是所有配方中最高的，并且因其丙烯酸酯结构，双键周围没有甲基支链，双键反应活性较高，所以此配方的转化率最高，固化效果最好，达到83.08%，可以确认固化程度较高。光引发剂对固化程度也有较大的影响，总体来看，光引发剂184的总体固化程度较高，表现出更高的引发效率。
固化转化率主要和单体与引发剂的种类有关，EDG在所有单体中的转化率偏低，这主要是由于丙烯酸甲酯结构中的甲基侧链会影响双键的交联结构，导致该单体的转化率整体偏低。
2.3 UV固化树脂的热力学性能
通过DSC扫描测试对10种油墨配方经过UV固化与热固化后的热力学性能进行测试，并将所有固化后样品的玻璃化转变温度列于表3中。从表3可以看出，固化后树脂的Tg普遍较高，且高于常规丙烯酸酯类聚合物，这主要是因双官能度单体固化后提高了体系的交联密度，同时引入了杂萘联苯等刚性基团，使得分子的内旋转受阻，提高了聚合物的耐热性。其中TGD油墨配方的Tg较高，这主要是由于双键旁的丙烯酸酯类取代基体积较大，分子内旋转受阻，导致了Tg的升高。
在光固化过程中，由于两种光引发剂活性不同，双丙烯酸酯基团中的接枝、共聚、嵌段等反应程度差异较大，从而引起固化程度不同。图5为PTED与PEDG体系的DSC曲线，通过对比PTGD与PEDG体系的Tg，光引发剂184的油墨配方所制备的聚合物Tg更高，表明光引发剂184固化物的固化反应程度较高，该结果与红外测试数据一致。
通过TGA测试不同UV固化油墨体系的热稳定性，测得5%热分解温度（Td5%）结果如表3所示。固化物的热失重温度主要与单体的分子结构与交联程度有关。由于HD单体内的醚键含量最少，分子间的交联程度高，其体系的Td5%在所有油墨中最高，高达370℃。EDG体系固化后的转化率仅有50%～65%，交联程度过低，因此其制备的油墨Td5%在所有油墨中最低，仅有270℃。
2.4 UV固化油墨的固化收缩率
UV油墨固化后，分子内的双键被打开，分子之间通过共价键链接，导致了体积的收缩，同时因为分子间固化后形成交联体系，分子链的自由运动被限制，使得固化后体积收缩[13]。选取光引发剂184作为引发剂，实验测得不同方式固化后树脂的收缩率如表4所示。从表4可以看出，除了NGD油墨体系，其他UV油墨固化体系的固化收缩率均未高于5%，展现了良好的尺寸稳定性。
2.5 UV固化油墨的力学性能
选取光引发剂184作为拉伸测试样品的引发剂，探究活性稀释剂单体的选择对于力学性能的影响，得到不同UV固化树脂薄膜的力学性能测试结果如表5所示，从表5可以看出，PTED184树脂具有最高的弹性模量和拉伸强度，这主要是由于其分子链排列过为规整，聚合物内自由体积较小，分子链段的运动受阻，导致其柔韧性变差。NGD油墨体系固化后的弹性模量最低但其断裂伸长率最高，呈现出软而弱的力学特性，与其分子链的柔性有关。
2.6 UV固化油墨的介电性能
光引发剂184固化后的样品介电性能测试结果如表6所示。从表6可以看出，由TGD单体所配置的油墨配方的介电性能最好。在10 GHz测试频率下，介电常数（Dk）和介质损耗因数（Df）最低，分别为2.61和0.014。这是由于其体系极性低，链段柔性大，易交联缠结从而限制链段的运动。当单体中醚键的含量增多时，油墨在固化后的介电性能较差，这是由于醚键相对于脂肪链的极性较强，使材料的介电常数增大。随着介电测试的频率由10 GHz提升至28 GHz时，光固化薄膜的介电常数均有所增加，增大幅度为0～9.5%。这是由于在28 GHz的中高频率下，分子链侧基运动增强，导致介电常数上升。其中PNGD184的介电常数变化相对较大，这可能是由于其侧基较多造成的[14-15]。
3 结论
收起
针对3D打印油墨配方研究，分别选用了5种活性稀释剂，对油墨的3D打印固化工艺进行比较，并对固化后树脂的力学性能、耐热性能和介电性能进行测试，得出以下结论：
（1）经过红外固化程度测试，NGD油墨体系的固化程度最高，达85%以上。
（2）通过DSC与TGA进行热力学性能测试，固化后TGD油墨体系的Tg最高可达210℃，且使用光引发剂184的UV固化油墨的Tg相比于光引发剂907的高。
（3）介电性能测试表明，在10 GHz测试频率下，所有油墨体系固化后的介电常数均较低，介质损耗因数未高于0.04。
综上，可选用NGD或TGD为活性稀释剂，光引发剂184为引发剂，FPPE聚芳醚齐聚物树脂为预聚物作为3D油墨的三大主要配方，制备得到的树脂具有较优良的综合性能，具备在微电子领域应用的前景。
基金
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  • 国家自然科学基金青年科学基金资助项目(51903028)
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2024年第57卷第8期
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doi: 10.16790/j.cnki.1009-9239.im.2024.08.005
  • 接收时间：2023-05-14
  • 首发时间：2025-12-24
  • 出版时间：2024-08-20
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  • 收稿日期：2023-05-14
  • 修回日期：2024-04-22
基金
国家自然科学基金青年科学基金资助项目(51903028)
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    中国电子科技集团公司第十研究所，四川 成都 610036
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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
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total species (%)		 属
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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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