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Article(id=1239133501031764041, tenantId=1146029695717560320, journalId=1238841944844054536, issueId=1239133496480953194, articleNumber=null, orderNo=null, doi=10.12347/j.ycyk.20241210004, pmid=null, cstr=32406.14.ycyk.20241210004, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1733760000000, receivedDateStr=2024-12-10, revisedDate=1735228800000, revisedDateStr=2024-12-27, acceptedDate=null, acceptedDateStr=null, onlineDate=1773362048633, onlineDateStr=2026-03-13, pubDate=1747238400000, pubDateStr=2025-05-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773362048633, onlineIssueDateStr=2026-03-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773362048633, creator=13701087609, updateTime=1773362048633, updator=13701087609, issue=Issue{id=1239133496480953194, tenantId=1146029695717560320, journalId=1238841944844054536, year='2025', volume='46', issue='3', pageStart='1', pageEnd='152', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773362047547, creator=13701087609, updateTime=1773363045127, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1239137680697651401, tenantId=1146029695717560320, journalId=1238841944844054536, issueId=1239133496480953194, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1239137680697651402, tenantId=1146029695717560320, journalId=1238841944844054536, issueId=1239133496480953194, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=63, endPage=69, ext={EN=ArticleExt(id=1239133501287616593, articleId=1239133501031764041, tenantId=1146029695717560320, journalId=1238841944844054536, language=EN, title=Packaging and Performance Study of Polymer Derived Ceramics Thin-Film Thermocouples, columnId=1239133497370145646, journalTitle=Journal of Telemetry, Tracking and Command, columnName=Intelligent Sensor Technology, runingTitle=null, highlight=null, articleAbstract=

Polymer Derived Ceramics (PDCs) thin-film thermocouples have the advantages of a simple preparation process and a stable high-temperature performance. They are very suitable for temperature measurement of hot-end components such as aircraft engine turbine blades. However, as the operating temperature of advanced engines increases, the upper limit of their temperature resistance needs to be improved. This article develops a precursor ceramic encapsulated PDCs: ITO/In2O3 thin film thermocouple. The encapsulation layer uses SiCN as the precursor solution and nano-Al2O3 powder as the filling material, and is prepared by the screen printing process. High-temperature test results show that the prepared sensor can survive at 1 500 °C in the short term and have stable output within 1 400 °C. The calibration test at 1 100 °C shows a linearity better than 0.999, with a multiple-cycle error of less than 1%.

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先驱体陶瓷（Polymer Derived Ceramics，PDCs）薄膜热电偶具有制备工艺简单、高温性能稳定等优点，非常适用于给航空发动机涡轮叶片等热端部件测温，但随着先进发动机工作温度的不断提升，其耐温上限亟待进一步提高。本文开发了一款先驱体陶瓷封装的PDCs：ITO/In2O3薄膜热电偶，其封装层以SiCN为先驱体溶液、纳米Al2O3粉末为填充材料，采用丝网印刷工艺制备。高温测试结果表明：所制备的传感器能够在短期内于1 500 ℃环境下正常工作，并在1 400 ℃内有稳定的信号输出；在1 100 ℃下进行标定测试，其线性度优于0.999，多次循环误差小于1%。

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陈沁楠（）
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张朋　1999年生，硕士研究生。

陈沁楠　1987年生，博士，副教授，博士生导师。

徐毅　1987年生，博士研究生，研究员。

李金洋　1988年生，博士，研究员。

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张朋　1999年生，硕士研究生。

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张朋　1999年生，硕士研究生。

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陈沁楠　1987年生，博士，副教授，博士生导师。

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陈沁楠　1987年生，博士，副教授，博士生导师。

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3中国航发四川燃气涡轮研究院 绵阳 621000, bio={"content":"

徐毅　1987年生，博士研究生，研究员。

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徐毅　1987年生，博士研究生，研究员。

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李金洋　1988年生，博士，研究员。

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李金洋　1988年生，博士，研究员。

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language=CN, label=图7, caption=带保护层热电偶的标定测试, figureFileSmall=8ckU7onZHB48TQ1TcaF9kA==, figureFileBig=1etnpisfiHGv31t3rq/Ljg==, tableContent=null), ArticleFig(id=1239263570215629113, tenantId=1146029695717560320, journalId=1238841944844054536, articleId=1239133501031764041, language=EN, label=Fig.8, caption=High-temperature test signals, figureFileSmall=Aw3vTikRd8qM10+O5r306A==, figureFileBig=qxPdHYcqmS0QSMGPef3udA==, tableContent=null), ArticleFig(id=1239263570307903805, tenantId=1146029695717560320, journalId=1238841944844054536, articleId=1239133501031764041, language=CN, label=图8, caption=高温测试信号, figureFileSmall=Aw3vTikRd8qM10+O5r306A==, figureFileBig=qxPdHYcqmS0QSMGPef3udA==, tableContent=null), ArticleFig(id=1239263570379206979, tenantId=1146029695717560320, journalId=1238841944844054536, articleId=1239133501031764041, language=EN, label=Table 1, caption=

Three-round test data of the thin-film thermocouples with the protective layer

, figureFileSmall=null, figureFileBig=null, tableContent=
次数/温度400 ℃600 ℃800 ℃1 000 ℃1 100 ℃
1/(mV)37.5662.2788.88114.59127.64
2/(mV)37.2562.7588.51113.607126.43
3/(mV)37.8462.4089.45114.98127.97
最大误差0.745%0.77%0.641%-0.857%0.258%
), ArticleFig(id=1239263570475675977, tenantId=1146029695717560320, journalId=1238841944844054536, articleId=1239133501031764041, language=CN, label=表1, caption=

带保护层热电偶三轮测试数据

, figureFileSmall=null, figureFileBig=null, tableContent=
次数/温度400 ℃600 ℃800 ℃1 000 ℃1 100 ℃
1/(mV)37.5662.2788.88114.59127.64
2/(mV)37.2562.7588.51113.607126.43
3/(mV)37.8462.4089.45114.98127.97
最大误差0.745%0.77%0.641%-0.857%0.258%
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先驱体陶瓷薄膜热电偶的封装及性能研究
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张朋 1 , 陈沁楠 1 , 徐毅 2, 3 , 李金洋 4
遥测遥控 | 智能传感器技术 2025,46(3): 63-69
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遥测遥控 | 智能传感器技术 2025, 46(3): 63-69
先驱体陶瓷薄膜热电偶的封装及性能研究
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张朋1, 陈沁楠1 , 徐毅2, 3, 李金洋4
作者信息
  • 1厦门大学 厦门 361005
  • 2北京航空航天大学 北京 100191
  • 3中国航发四川燃气涡轮研究院 绵阳 621000
  • 4北京遥测技术研究所 北京 100076

    • 张朋　1999年生，硕士研究生。

    陈沁楠　1987年生，博士，副教授，博士生导师。

    徐毅　1987年生，博士研究生，研究员。

    李金洋　1988年生，博士，研究员。

通讯作者:

陈沁楠（）
Packaging and Performance Study of Polymer Derived Ceramics Thin-Film Thermocouples
Peng ZHANG1, Qinnan CHEN1 , Yi XU2, 3, Jinyang LI4
Affiliations
  • 1.Xiamen University, Xiamen 361005, China
  • 2.Beijing University of Aeronautics and Astronautics, Beijing 100191, China
  • 3.AECC Sichuan Gas Turbine Establishment, Mianyang 621000, China
  • 4.Beijing Research Institute of Telemetry, Beijing 100076, China
出版时间: 2025-05-15 doi: 10.12347/j.ycyk.20241210004
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摘要
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先驱体陶瓷（Polymer Derived Ceramics，PDCs）薄膜热电偶具有制备工艺简单、高温性能稳定等优点，非常适用于给航空发动机涡轮叶片等热端部件测温，但随着先进发动机工作温度的不断提升，其耐温上限亟待进一步提高。本文开发了一款先驱体陶瓷封装的PDCs：ITO/In2O3薄膜热电偶，其封装层以SiCN为先驱体溶液、纳米Al2O3粉末为填充材料，采用丝网印刷工艺制备。高温测试结果表明：所制备的传感器能够在短期内于1 500 ℃环境下正常工作，并在1 400 ℃内有稳定的信号输出；在1 100 ℃下进行标定测试，其线性度优于0.999，多次循环误差小于1%。

先驱体陶瓷  /  ITO/In2O3  /  高温封装  /  极端环境

Polymer Derived Ceramics (PDCs) thin-film thermocouples have the advantages of a simple preparation process and a stable high-temperature performance. They are very suitable for temperature measurement of hot-end components such as aircraft engine turbine blades. However, as the operating temperature of advanced engines increases, the upper limit of their temperature resistance needs to be improved. This article develops a precursor ceramic encapsulated PDCs: ITO/In2O3 thin film thermocouple. The encapsulation layer uses SiCN as the precursor solution and nano-Al2O3 powder as the filling material, and is prepared by the screen printing process. High-temperature test results show that the prepared sensor can survive at 1 500 °C in the short term and have stable output within 1 400 °C. The calibration test at 1 100 °C shows a linearity better than 0.999, with a multiple-cycle error of less than 1%.

Polymer derived ceramics  /  ITO/In2O3  /  High temperature packaging  /  Extreme environments
张朋, 陈沁楠, 徐毅, 李金洋. 先驱体陶瓷薄膜热电偶的封装及性能研究. 遥测遥控, 2025 , 46 (3) : 63 -69 . DOI: 10.12347/j.ycyk.20241210004
Peng ZHANG, Qinnan CHEN, Yi XU, Jinyang LI. Packaging and Performance Study of Polymer Derived Ceramics Thin-Film Thermocouples[J]. Journal of Telemetry, Tracking and Command, 2025 , 46 (3) : 63 -69 . DOI: 10.12347/j.ycyk.20241210004
正文
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0　引言
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随着航空航天技术的快速发展，发动机热端部件面临更大的热流冲击。其中，第四代航空发动机涡轮进口温度超过2 000 K，发动机内部热力监测尤其是涡轮叶片等热端部件的温度监测需求对传感器高温存活性能提出了更大的挑战[1,2]。另外，不断提升高温传感器的测温上限有利于人类探索未知领域，因此提升高温传感器的极端环境耐受性和使用寿命至关重要。高温薄膜热电偶以其对流场无干扰、原位感知、结构简单等优势被广泛地研究[3-5]。
近年来，高温薄膜热电偶研究主要集中在Pt-Rh以及Pt组成的贵金属薄膜热电偶，尽管具有高熔点，但金属薄膜热电偶在高温下容易氧化使得传感器长期稳定性较差[6-10]，与金属薄膜热电偶相比陶瓷薄膜热电偶表现出强的耐温特性以及优异的热电特性，其中ITO/In2O3热电偶由于输出热电势大、耐温上限高、输出信号稳定、抗干扰性强被广泛的关注[11-14]。2017年，赵晓辉等人在氮气氛围下制备了氮气掺杂的ITO/In2O3热电偶，提高了薄膜的线性度和高温稳定性，但其塞贝克系数下降至64.7 μV/℃[15]；2019年，刘丹等人通过溅射Al2O3制备保护层的工艺来提高ITO/In2O3热电偶的高温性能，虽然抑制了膜层的挥发使得传感器可以在1 250 ℃下测试10 h，但是仍然有较大的漂移率，且制备工艺复杂[16]；2023年，陈沁楠等人采用先驱体陶瓷掺杂的方式制备出PDCs: ITO/In2O3薄膜热电偶，制备工艺简单，可以实现1 200 ℃下的高精度测量，稳定性优于1 ℃/h[17]，但其测量耐温上限仍有待提升。
本文报道了一种先驱体陶瓷封装的PDCs: ITO/In2O3薄膜热电偶，以Al2O3纳米粉末为陶瓷先驱体改性填料，采用丝网印刷工艺制备，减少保护层的制备周期，采用维森堡直写工艺制备敏感层；对在Al2O3基底制备的具有先驱体陶瓷封装的PDCs: ITO/In2O3薄膜热电偶进行性能测试，结果表明所制备的热电偶可以在1 500 ℃下短暂存活，在1 400 ℃及以下有较为稳定的信号，在检定炉中测试，表现出良好的再现性、稳定性及精度，展现了该传感器在高温监测特别是航空发动机热端部件健康监测方面重要的潜力。
1　测试原理及传感器结构
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1.1　材料
采用粒径为50 nm的Al2O3粉末为保护层陶瓷先驱体填充材料，采用中科院化学研究所的PSN2为制备各膜层所需的先驱体溶液，采用粒径为1 μm的ITO以及In2O3作为敏感层填充材料，采用深圳市塞雅电子浆料有限公司的浆料稀释剂调节溶液粘度，薄膜热电偶的绝缘基板为96% Al2O3片，Rz为0.8 μm。
1.2　制备流程
制备流程如图1所示，将PSN2溶液与粒径为50 nm的氧化铝粉末以及粒径为1 μm的ITO以及In2O3粉末按照质量分数比为1:2、1:4、1:4的方式混合掺杂，并且放置于磁力搅拌机上搅拌，搅拌时长为3 h，根据溶液的粘稠度和后续实验的需要，在流动性过低的混合溶液中加入定量的浆料稀释剂提高流动性。将基底放入酒精中进行超声波清洗，并进行干燥处理，将所制备带有ITO和In2O3的先驱体溶液注入维森堡直写设备的储液空腔内，在基底上制备热电偶两电极，电极的长度为100 mm，宽度为600 μm，将制备完成的器件进行300 ℃、2 h的固化，再以4 ℃/min的升温速度升到1200 ℃，保温1 h并以4 ℃/min的速率降至室温，完成敏感层制备。采用50 μm厚的丝网印刷掩膜，将氧化铝保护层预制浆料涂敷于所制备的热电偶表面，在空气中200 ℃对其进行预固化处理，预固化时间为1 h。将上述所制备的器件放置于管式炉中进行高温退火，退火参数为：升温速度为8 ℃/min，升温到1 200 ℃，保温1 h，随后以10 ℃/min的速度进行降温，降低至室温，如图2(a)所示，由于液态向固态转变产生收缩的现象，所以在1 200 ℃初步退火后，在保护层的表面会出现大量的裂纹，裂纹的存在会极大的影响对敏感层的密封保护，降低保护能力。为了降低裂纹对保护层的影响，将传感器进行高温老化处理，老化参数为：将传感器放置在高温管式炉中，进行1 300 ℃ 4 h的保温处理，在1 300 ℃时氧化硅会成为液态，其流动性会带动氧化铝粉末移动，将缝隙进行填补，实现保护层的密封处理，如图2(b)所示，高温老化后保护层致密无明显裂纹。
1.3　测试原理
薄膜热电偶的测试示意图如图3所示。为了评估热电偶输出电势，将热电偶的一端插入高温检定炉中，另外一端固定在水冷平台上，热电偶冷端外接导线和两个标准热电偶连接到数据采集卡上，并且连接到PC端实时显示，冷热端测温可靠。热电响应与温差之间的关系如式(1)所示[18]：
式中，ΔT为热结点和冷端之间的温度差，A、B和C是可通过多项式拟合获得的常数。D设置为0以满足边界条件。
薄膜热电偶的精度至关重要，根据薄膜热电偶的温度测量原理，精度AC的计算公式如公式(2)所示[19,20]：
式中ΔT'表示通过曲线计算的温差，ΔT表示通过实验测试获得的温差，Th表示热端的最高温度，AC表示温差ΔT对应的精度。
1.4　所用设备
采用扫描电子显微镜和能谱仪(SEM–Mapping，SUPRA55 SAPPHIRE，Carl Zeiss，Germany)分别测量膜层的形貌和元素分析。采用X射线衍射仪(XRD，MAXima X XRD-7000)测定样品的晶体结构。使用Keysight 34972A数据采集系统(DAQ，Data Acquisition System)在管式炉中测量薄膜热电偶的电动势。热结点处使用商用B型热电偶监测温度，冷结点处采用商业K型热电偶监测温度。
2　测试与讨论
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2.1　膜层表征
图4所示为带有保护层的热电偶结构示意图。在氧化铝基底上制备的器件的截面表征如图5所示。从图中可以看出制备的带有保护层的器件，各膜层致密、有明显界限，在高温下没有互相溶解渗透的现象，这在一定程度上保证了所制备的器件在高温下的可靠性，以及测试过程中信号的稳定，所制备的器件敏感层的厚度为17 μm，保护层的厚度为41 μm，足够厚的保护层实现可靠的空气阻隔，通过EDS可以看出所制备的膜层主要有Al、N、O、C、In、Sn、Si等元素，其中相关导电元素均存在于中间敏感层，N、O、C各膜层均含有。
2.2　性能测试
对所制备带有保护层的热电偶进行耐高温信号测试，在1 200 ℃、1 300 ℃、1 400 ℃以及1 500 ℃下保温1 h，通过截面电镜去测量敏感层的厚度变化与没有带保护层的热电偶进行对比如图6(a)所示，可以看出随着温度的上升热电偶的敏感层都出现了挥发的趋势，其中对于没有保护层的热电偶进行分析，随着温度的升高其敏感层的衰减速度逐渐变快，在1 500℃下衰减到原有膜层的23.6%，膜层产生剧烈的挥发，对于带有保护层热电偶其敏感层的挥发速度远小于不带保护层，虽然随着温度的升高，其膜层的厚度也有一个衰减的趋势，但是最终保持在原有膜层的80%左右，证明所制备的陶瓷保护层极大抑制了热电偶敏感层的挥发；测量带有保护层的热电偶在各温度段下有无稳定的信号输出，如图6(b)所示，随着温度的升高，热电偶都具有一个良好的输出响应，在1 500℃下热电偶的输出波动较大，但是可以明显的看出在输出波动较大的1 500℃下的响应其大部的数据点依旧稳定在一个范围内，具有明显的响应输出，在该温度段内的输出噪声较大可能是由于在1 500℃时，敏感层出现液化现象，致使输出信号产生强烈的波动。
将热电偶放置于检定炉中进行标定测试，选取五个温度点：400 ℃、600 ℃、800 ℃、1 000 ℃以及1 100 ℃下进行的三轮测试标定，以第一轮测试数据标定，在各温度段各选择一个输出电势信号点共五个信号点，分别为37.65 mV、62.27 mV、88.88 mV、114.59 mV、127.64 mV。根据热电偶的计算公式，此时横坐标为高低温的温度差，将五个信号点进行一次线性拟合和三次线性拟合，如图7所示，其中通过一次拟合所得出的拟合度为0.999 52，通过三次拟合所得出的拟合度为0.999 62，均表现出极佳的拟合度，通过拟合得知所制备的带有保护层的热电偶的平均输出塞贝克系数为141 μV/℃。
将传感器进行三轮测试，如图8(a)~图8(c)所示，带有保护层的热电偶具有优异的重复性，见表1。在三轮测试中，当高温区域为400 ℃时，三轮测试的电学信号为37.56 mV、37.25 mV、37.84 mV；高温区域为600 ℃时，三轮测试的电学信号为62.27 mV、62.75 mV、62.40 mV；高温区域为800 ℃时，三轮测试的电学信号为88.88 mV、88.51 mV、89.45 mV；高温区域为1 000 ℃时，三轮测试的电学信号为114.59 mV、113.607 mV、114.98 mV；高温区域为1 100 ℃时，三轮测试的电学信号为127.64 mV、126.43 mV、127.97 mV。以第一轮测试为标准，计算三轮测试的最大误差，通过计算得出在热点温度为400、600、800、1 000以及1 100 ℃时三轮测试的最大误差分别为0.745%、0.77%、0.641%、-0.857%以及0.258%，可以看出三轮测试中最大的测试误差为-0.857%，如图8(d)所示，进行多轮循环测试传感器具有良好的一致性及信号反映。
3　结束语
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针对薄膜热电偶耐温上限低、容易被氧化等问题，本文开发了一种具有先驱体陶瓷封装的PDCs: ITO/In2O3薄膜热电偶，采用Al2O3纳米粉末为陶瓷先驱体改性填料，使用丝网印刷工艺制备保护层，所制备的带有保护层的薄膜热电偶可以在1 500 ℃下存活，在1 100 ℃内进行标定测试，得出传感器的平均塞贝克系数为141 μV/℃，三次线性拟合度为0.999 62，具有极佳的线性度。多轮循环测试，得出测试误差小于1%。综上，所制备的具有先驱体陶瓷封装工艺的PDCs: ITO/In2O3薄膜热电偶具有耐高温、精度高、线性度强等优势，有望应用于极端高温环境温度测试如航空发动机热端健康监测。
基金
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  • 国家科技重大专项(J2019-V-0015-0110)
  • 国家自然科学基金(62475224)
文献
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doi: 10.12347/j.ycyk.20241210004
  • 接收时间：2024-12-10
  • 首发时间：2026-03-13
  • 出版时间：2025-05-15
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  • 收稿日期：2024-12-10
  • 修回日期：2024-12-27
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国家科技重大专项(J2019-V-0015-0110)
国家自然科学基金(62475224)
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    1厦门大学 厦门 361005
    2北京航空航天大学 北京 100191
    3中国航发四川燃气涡轮研究院 绵阳 621000
    4北京遥测技术研究所 北京 100076

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陈沁楠（）
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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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