<?xml version="1.0" encoding="UTF-8"?>
<!DOCTYPE article PUBLIC "-//NLM//DTD JATS (Z39.96) Journal Publishing DTD v1.3 20210610//EN" "JATS-journalpublishing1-3.dtd">
<article article-type="research-article" dtd-version="1.3" xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns:xsi="http://www.w3.org/2001/XMLSchema-instance" xml:lang="ru"><front><journal-meta><journal-id journal-id-type="publisher-id">zldm</journal-id><journal-title-group><journal-title xml:lang="ru">Заводская лаборатория. Диагностика материалов</journal-title><trans-title-group xml:lang="en"><trans-title>Industrial laboratory. Diagnostics of materials</trans-title></trans-title-group></journal-title-group><issn pub-type="ppub">1028-6861</issn><issn pub-type="epub">2588-0187</issn><publisher><publisher-name>ООО «Издательство «ТЕСТ-ЗЛ»</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.26896/1028-6861-2024-90-8-47-54</article-id><article-id custom-type="elpub" pub-id-type="custom">zldm-2272</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Article</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="ru"><subject>ИССЛЕДОВАНИЕ СТРУКТУРЫ И СВОЙСТВ. ФИЗИЧЕСКИЕ МЕТОДЫ ИССЛЕДОВАНИЯ И КОНТРОЛЯ</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="en"><subject>TESTING OF STRUCTURE AND PARAMETERS. PHYSICAL METHODS OF TESTING AND QUALITY CONTROL</subject></subj-group></article-categories><title-group><article-title>Определение температуры стеклования электротехнических препрегов методом ДСК</article-title><trans-title-group xml:lang="en"><trans-title>Determination of the glass transition temperature of electrotechnical prepregs by differential scanning calorimetry (DSC)</trans-title></trans-title-group></title-group><contrib-group><contrib contrib-type="author" corresp="yes"><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Карезин</surname><given-names>К. И.</given-names></name><name name-style="western" xml:lang="en"><surname>Karezin</surname><given-names>Konstantin I.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Константин Игоревич Карезин, </p><p>127030, Москва, ул. Сущевская, д. 22. </p></bio><bio xml:lang="en"><p>Konstantin I. Karezin, </p><p>22, ul. Sushchevskaya, Moscow, 127030</p></bio><email xlink:type="simple">mailbox75@vniia.ru</email><xref ref-type="aff" rid="aff-1"/></contrib><contrib contrib-type="author" corresp="yes"><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Попова</surname><given-names>Е. И.</given-names></name><name name-style="western" xml:lang="en"><surname>Popova</surname><given-names>Ekaterina I.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Екатерина Ивановна Попова, </p><p>127030, Москва, ул. Сущевская, д. 22.</p></bio><bio xml:lang="en"><p>Ekaterina I. Popova, </p><p>22, ul. Sushchevskaya, Moscow, 127030</p></bio><xref ref-type="aff" rid="aff-1"/></contrib><contrib contrib-type="author" corresp="yes"><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Невский</surname><given-names>Р. Е.</given-names></name><name name-style="western" xml:lang="en"><surname>Nevskiy</surname><given-names>Roman E.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Роман Евгеньевич Невский, </p><p>127030, Москва, ул. Сущевская, д. 22.</p></bio><bio xml:lang="en"><p>Roman E. Nevskiy, </p><p>22, ul. Sushchevskaya, Moscow, 127030</p></bio><xref ref-type="aff" rid="aff-1"/></contrib><contrib contrib-type="author" corresp="yes"><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Соковишин</surname><given-names>А. В.</given-names></name><name name-style="western" xml:lang="en"><surname>Sokovishin</surname><given-names>Alexey V.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Алексей Владимирович Соковишин,</p><p>127030, Москва, ул. Сущевская, д. 22.</p></bio><bio xml:lang="en"><p>Alexey V. Sokovishin,</p><p>22, ul. Sushchevskaya, Moscow, 127030</p></bio><xref ref-type="aff" rid="aff-1"/></contrib></contrib-group><aff-alternatives id="aff-1"><aff xml:lang="ru"><institution>Всероссийский НИИ автоматики имени Н. Л. Духова (ФГУП «ВНИИА»)</institution><country>Россия</country></aff><aff xml:lang="en"><institution>Dukhov Automatics Research Institute (FSUE VNIIA)</institution><country>Russian Federation</country></aff></aff-alternatives><pub-date pub-type="collection"><year>2024</year></pub-date><pub-date pub-type="epub"><day>25</day><month>08</month><year>2024</year></pub-date><volume>90</volume><issue>8</issue><fpage>47</fpage><lpage>54</lpage><permissions><copyright-statement>Copyright &amp;#x00A9; Карезин К.И., Попова Е.И., Невский Р.Е., Соковишин А.В., 2024</copyright-statement><copyright-year>2024</copyright-year><copyright-holder xml:lang="ru">Карезин К.И., Попова Е.И., Невский Р.Е., Соковишин А.В.</copyright-holder><copyright-holder xml:lang="en">Karezin K.I., Popova E.I., Nevskiy R.E., Sokovishin A.V.</copyright-holder><license xml:lang="ru" license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>Данная работа распространяется под лицензией Creative Commons Attribution 4.0.</license-p></license><license xml:lang="en" license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>This work is licensed under a Creative Commons Attribution 4.0 License.</license-p></license></permissions><self-uri xlink:href="https://www.zldm.ru/jour/article/view/2272">https://www.zldm.ru/jour/article/view/2272</self-uri><abstract><p>Препреги электротехнического назначения используют в качестве склеивающей прокладки отдельных слоев при изготовлении многослойных печатных плат. Они представляют собой материалы, получаемые путем пропитки стеклоткани смесью модифицированных эпоксидных смол. Температуру стеклования (Tст) отвержденного препрега определяют методом дифференциальной сканирующей калориметрии. Данный подход универсален, предусматривает широкие границы инструментальных параметров и не содержит численных значений метрологических характеристик. В работе представлены методика определения Tст с учетом требований ГОСТа и условий проведения экспериментов и оценка ее метрологических характеристик. Исследовали отвержденные образцы препрегов российского и зарубежного производств. Термограммы записывали на двух пробах для каждого образца, Tст рассчитывали по переходу стеклования на кривой второго нагрева со скоростью 20 °C/мин. Показано, что относительная суммарная погрешность методики составляет ±4 %. Поскольку в отдельных случаях на термограммах отвержденных препрегов видимый переход стеклования не фиксировался, проводили линейную аппроксимацию зависимости Tст от высоких скоростей нагрева, при которых переход стеклования выражен заметно лучше, к значению скорости 20 °C/мин. Контроль правильности определения осуществляли на образцах, для которых можно было уверенно определить Tст экстраполяционным и классическим экспериментально-расчетным способами. Установлено, что оба метода расчета приводят к одинаковым результатам в пределах погрешности анализа. Полученные результаты могут быть использованы при определении Tст препрегов электротехнического назначения и входном контроле соответствующих изделий.</p></abstract><trans-abstract xml:lang="en"><p>Electrotechnical prepregs are used as gluing gasket in the manufacture of multilayer printed circuit boards. These materials are obtained by fiberglass impregnation with a mixture of modified epoxy resins. The glass transition temperature (Tg) of the cured prepreg is determined by differential scanning calorimetry. This universal approach provides a wide range of instrumental parameters and does not contain numerical values of metrological characteristics. We present a methodology of Tg determination taking into account the requirements of GOST and experimental conditions and assess the metrological characteristics of the technique. Cured samples of prepregs produced in Russia and aboard were studied. Thermograms were recorded for two samples of each prepreg. Tg was calculated from the transition on the curve of second heating at a rate of 20 °C/min. It has been shown that the relative total error of the method is ±4%. Since in some cases the visible glass transition was not recorded on the thermograms of cured prepregs, a linear approximation of the Tg dependence from a high heating rate at which the glass transition is more pronounced to the value of 20 °C/min was carried out. Control of the correctness of the determination was carried on samples for which Tg can be confidently determined by extrapolation and traditional experimental-calculation methods. It is shown that both extrapolation and calculation methods lead to the same results within the limits of the analytical error. The obtained results can be used for determining Tg of electrotechnical prepregs and incoming inspection of the corresponding product.</p></trans-abstract><kwd-group xml:lang="ru"><kwd>дифференциальная сканирующая калориметрия</kwd><kwd>электротехнические препреги</kwd><kwd>температура стеклования</kwd><kwd>степень отверждения</kwd><kwd>скорость нагрева</kwd><kwd>метрологические характеристики</kwd></kwd-group><kwd-group xml:lang="en"><kwd>differential scanning calorimetry</kwd><kwd>electrotechnical prepregs</kwd><kwd>glass transition temperature</kwd><kwd>degree of cure</kwd><kwd>heating rate</kwd><kwd>metrological characteristics</kwd></kwd-group><funding-group><funding-statement xml:lang="ru">Работа финансировалась за счет средств бюджета института (учреждения, организации).</funding-statement></funding-group></article-meta></front><back><ref-list><title>References</title><ref id="cit1"><label>1</label><citation-alternatives><mixed-citation xml:lang="ru">Xie C., Zou H., Wei-Yao., Wang M. Research on reliability of non-flow prepreg filling in automotive R-F PCB / 16th International microsystems, packaging, assembly and circuits technology conference (IMPACT). — Taipei, Taiwan, 2021. P. 82 – 85. DOI: 10.1109/IMPACT53160.2021.9697053</mixed-citation><mixed-citation xml:lang="en">Xie C., Zou H., Wei-Yao., Wang M. Research on reliability of non-flow prepreg filling in automotive R-F PCB / 16th International microsystems, packaging, assembly and circuits technology conference (IMPACT). — Taipei, Taiwan, 2021. P. 82 – 85. DOI: 10.1109/IMPACT53160.2021.9697053</mixed-citation></citation-alternatives></ref><ref id="cit2"><label>2</label><citation-alternatives><mixed-citation xml:lang="ru">Liu T., Devarajan M. Influence of prepreg material properties on printed circuit board stack-up / 72nd electronic components and technology conference (ECTC). IEEE. — San Diego, CA, USA, 2022. P. 2244 – 2248. DOI: 10.1109/ECTC51906.2022.00354</mixed-citation><mixed-citation xml:lang="en">Liu T., Devarajan M. Influence of prepreg material properties on printed circuit board stack-up / 72nd electronic components and technology conference (ECTC). IEEE. — San Diego, CA, USA, 2022. P. 2244 – 2248. DOI: 10.1109/ECTC51906.2022.00354</mixed-citation></citation-alternatives></ref><ref id="cit3"><label>3</label><citation-alternatives><mixed-citation xml:lang="ru">Бороздина Е. А. Методы испытания склеивающей прокладки, используемой для изготовления многослойных печатных плат. http://www.dnevnikinauki.ru/images/publications/2023/11/technics/Borozdina.pdf (дата обращения: 17.05.2024).</mixed-citation><mixed-citation xml:lang="en">Borozdina E. A. Methods of testing the adhesive gasket used for manufacture of multilayer printed circuit boards. http:// www.dnevnikinauki.ru/images/publications/2023/11/technics/Borozdina.pdf (accessed 17.05.2024) [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit4"><label>4</label><citation-alternatives><mixed-citation xml:lang="ru">Шимкин А. А., Сафронов А. М. Контроль качества полимерных связующих и препрегов методом ДСК / Заводская лаборатория. Диагностика материалов. 2016. Т. 82. № 8. С. 30 – 33.</mixed-citation><mixed-citation xml:lang="en">Shimkin A. A., Safronov A. M. Quality control of polymer binders by DSC / Industr. Lab. Mater. Diagn. 2016. Vol. 82. N 8. P. 30 – 33 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit5"><label>5</label><citation-alternatives><mixed-citation xml:lang="ru">Шимкин А. А., Гребенева Т. А., Меркулова Ю. И. Определение степени отверждения термореактивных связующих методами ИК-спектроскопии и дифференциальной сканирующей калориметрии / Заводская лаборатория. Диагностика материалов. 2017. Т. 83. № 8. С. 27 –32.</mixed-citation><mixed-citation xml:lang="en">Shimkin A. A., Grebneva T. A., Merkulova Yu. I. Determination of degree of cure of thermosetting resins using IR-spectroscopy and differential scanning calorimetry / Industr. Lab. Mater. Diagn. 2017. Vol. 83. N 8. P. 27 – 32 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit6"><label>6</label><citation-alternatives><mixed-citation xml:lang="ru">Макарова Н. Ю., Евстафьев С. С. Анализ отечественных материалов для производства печатных плат / Науч.-практ. конф. «Интеллектуальные системы и микросистемная техника»: сб. тр. — М.: МИЭТ, 2022. С. 283 – 291.</mixed-citation><mixed-citation xml:lang="en">Makarova N. Yu., Evstafev S. S. Analysis of domestic materials for the production of printed circuit boards / Research and practice conf. «Intelligent systems and microsystems engineering»: coll. of works. — Moscow: MIET, 2022. P. 283 – 291 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit7"><label>7</label><citation-alternatives><mixed-citation xml:lang="ru">Дубровский А. В., Егоров А. В. Вопросы расширения применения отечественных базовых материалов в изготовлении печатных плат / Электроника: наука, технология, бизнес. 2022. № 3(214). С. 160 – 165. DOI: 10.22184/1992-4178.2022.214.3.160.164</mixed-citation><mixed-citation xml:lang="en">Dubrovsky A. V., Egorov A. V. Concideration of expansion of domestic base materials implementation in bare boards production / Electronics: Science, Technology, Business. 2022. N 3(214). P. 160 – 165 [in Russian]. DOI: 10.22184/1992-4178.2022.214.3.160.164</mixed-citation></citation-alternatives></ref><ref id="cit8"><label>8</label><citation-alternatives><mixed-citation xml:lang="ru">Мурзин В. С., Нечипоренко Е. В., Котова С. В. и др. Дивинил-стирольные термоэластопласты как основа композиций / Каучук и резина. 2021. Т. 80. № 1. С. 16 – 19. DOI: 10.47664/0022-9466-2021-80-1-16-19</mixed-citation><mixed-citation xml:lang="en">Murzin V. S., Nechiporenko E. V., Kotova S. V., et al. Styrene-butadiene thermoplastics as the basis of adhesive compositions / Kauchuk Rez. 2021. Vol. 80. N 1. P. 16 – 19 [in Russian]. DOI: 10.47664/0022-9466-2021-80-1-16-19</mixed-citation></citation-alternatives></ref><ref id="cit9"><label>9</label><citation-alternatives><mixed-citation xml:lang="ru">Jiang J., Lu Z., Shen J., et al. Decoupling between calorimetric and dynamical glass transitions in high-entropy metallic glasses / Nature Commun. 2021. Vol. 12. P. 3843 – 3851. DOI: 10.1038/s41467-021-24093-w</mixed-citation><mixed-citation xml:lang="en">Jiang J., Lu Z., Shen J., et al. Decoupling between calorimetric and dynamical glass transitions in high-entropy metallic glasses / Nature Commun. 2021. Vol. 12. P. 3843 – 3851. DOI: 10.1038/s41467-021-24093-w</mixed-citation></citation-alternatives></ref><ref id="cit10"><label>10</label><citation-alternatives><mixed-citation xml:lang="ru">Хамидуллин О. Л., Мадиярова Г. М., Резвых А. В. и др. Сравнительный анализ термического расширения и теплоемкости полимеров на основе ряда эпоксиноволачных смол в широком диапазоне температур / Вестник технологического университета. 2021. Т. 24. № 5. С. 40 – 44.</mixed-citation><mixed-citation xml:lang="en">Khamidullin O. L., Madiyarova G. M., Rezvykh A. V., et al. Comparative analysis of thermal expansion and thermal capacity of polymers based on a series of epoxy novolak resins in a wide range of temperatures / Vestn. Tekhnol. Univ. 2021. Vol. 24. N 5. P. 40 – 44 [in Russian].</mixed-citation></citation-alternatives></ref><ref id="cit11"><label>11</label><citation-alternatives><mixed-citation xml:lang="ru">Van Miltenburg J. C., Cuevas-Diarte M. A. The influence of sample mass, heating rate and heat transfer coefficient on the form of DSC curves / Thermochim. Acta. 1989. Vol. 156. P. 291 – 297. DOI: 10.1016/0040-6031(89)87197-7</mixed-citation><mixed-citation xml:lang="en">Van Miltenburg J. C., Cuevas-Diarte M. A. The influence of sample mass, heating rate and heat transfer coefficient on the form of DSC curves / Thermochim. Acta. 1989. Vol. 156. P. 291 – 297. DOI: 10.1016/0040-6031(89)87197-7</mixed-citation></citation-alternatives></ref><ref id="cit12"><label>12</label><citation-alternatives><mixed-citation xml:lang="ru">Gaisford S. Fast-scan differential scanning calorimetry / Eur. Pharm. Rev. 2008. Vol. 4. P. 83 – 89.</mixed-citation><mixed-citation xml:lang="en">Gaisford S. Fast-scan differential scanning calorimetry / Eur. Pharm. Rev. 2008. Vol. 4. P. 83 – 89.</mixed-citation></citation-alternatives></ref><ref id="cit13"><label>13</label><citation-alternatives><mixed-citation xml:lang="ru">Gabbott P. V. Fast Scanning DSC / Principles and Applications of Thermal Analysis. — Wiley Blackwell, 2007. DOI: 10.1002/9780470697702.ch2</mixed-citation><mixed-citation xml:lang="en">Gabbott P. V. Fast Scanning DSC / Principles and Applications of Thermal Analysis. — Wiley Blackwell, 2007. DOI: 10.1002/9780470697702.ch2</mixed-citation></citation-alternatives></ref><ref id="cit14"><label>14</label><citation-alternatives><mixed-citation xml:lang="ru">Ford J. L., Mann T. E. Fast-Scan DSC and its role in pharmaceutical physical form characterization and selection / Advanced Drug Delivery Reviews. 2012. Vol. 64. P. 422 – 430. DOI: 10.1016/j.addr.2011.12.001</mixed-citation><mixed-citation xml:lang="en">Ford J. L., Mann T. E. Fast-Scan DSC and its role in pharmaceutical physical form characterization and selection / Advanced Drug Delivery Reviews. 2012. Vol. 64. P. 422 – 430. DOI: 10.1016/j.addr.2011.12.001</mixed-citation></citation-alternatives></ref><ref id="cit15"><label>15</label><citation-alternatives><mixed-citation xml:lang="ru">The handbook of differential scanning calorimetry. Techniques, instrumentation, inorganic and pharmaceutical substances. — Oxford: Elsevier, 2023. — 853 p. DOI: 10.1016/C2015-0-05607-6</mixed-citation><mixed-citation xml:lang="en">The handbook of differential scanning calorimetry. Techniques, instrumentation, inorganic and pharmaceutical substances. — Oxford: Elsevier, 2023. — 853 p. DOI: 10.1016/C2015-0-05607-6</mixed-citation></citation-alternatives></ref><ref id="cit16"><label>16</label><citation-alternatives><mixed-citation xml:lang="ru">McGregor C., Bines E. The use of high-speed differential scanning calorimetry (Hyper-DSC) in the study of pharmaceutical polymorphs / International Journal of Pharmaceutics. 2008. Vol. 350. P. 48 – 52. DOI: 10.1016/j.ijpharm.2007.08.015</mixed-citation><mixed-citation xml:lang="en">McGregor C., Bines E. The use of high-speed differential scanning calorimetry (Hyper-DSC) in the study of pharmaceutical polymorphs / International Journal of Pharmaceutics. 2008. Vol. 350. P. 48 – 52. DOI: 10.1016/j.ijpharm.2007.08.015</mixed-citation></citation-alternatives></ref><ref id="cit17"><label>17</label><citation-alternatives><mixed-citation xml:lang="ru">Poel G. V., Mathot V. B. F. High performance differential scanning calorimetry (HPer DSC): a powerful analytical tool for the study of the metastability of polymers / Thermochim. Acta. 2007. Vol. 461. P. 107 – 121. DOI: 10.1016/j.tca.2007.04.009</mixed-citation><mixed-citation xml:lang="en">Poel G. V., Mathot V. B. F. High performance differential scanning calorimetry (HPer DSC): a powerful analytical tool for the study of the metastability of polymers / Thermochim. Acta. 2007. Vol. 461. P. 107 – 121. DOI: 10.1016/j.tca.2007.04.009</mixed-citation></citation-alternatives></ref><ref id="cit18"><label>18</label><citation-alternatives><mixed-citation xml:lang="ru">Liu P., Yu L., Liu H., et al. Glass transition temperature of starch studied by a high-speed DSC / Carbohydrate Polymers. 2009. Vol. 77. P. 250 – 253. DOI: 10.1016/carbopol.2008.12.027</mixed-citation><mixed-citation xml:lang="en">Liu P., Yu L., Liu H., et al. Glass transition temperature of starch studied by a high-speed DSC / Carbohydrate Polymers. 2009. Vol. 77. P. 250 – 253. DOI: 10.1016/carbopol.2008.12.027</mixed-citation></citation-alternatives></ref></ref-list><fn-group><fn fn-type="conflict"><p>The authors declare that there are no conflicts of interest present.</p></fn></fn-group></back></article>
