WO2018214466A1 - 一种基于微纳荧光颗粒的薄膜热导率测量方法 - Google Patents

一种基于微纳荧光颗粒的薄膜热导率测量方法 Download PDF

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WO2018214466A1
WO2018214466A1 PCT/CN2017/114959 CN2017114959W WO2018214466A1 WO 2018214466 A1 WO2018214466 A1 WO 2018214466A1 CN 2017114959 W CN2017114959 W CN 2017114959W WO 2018214466 A1 WO2018214466 A1 WO 2018214466A1
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micro
nano fluorescent
film
tested
nano
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陈小源
张武康
方小红
李东栋
陈海燕
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中国科学院上海高等研究院
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

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  • the invention belongs to the field of micro-nano scale thermal coefficient measurement, and particularly relates to a method for measuring thermal conductivity of a film based on micro-nano fluorescent particles.
  • thermal conductivity In high-tech fields such as microelectronics, thin film materials are indispensable in the design and fabrication of MEMS and microelectronic devices, while thermal parameters such as thermal conductivity, specific heat and thermal diffusivity of thin film materials determine device and integrated circuit. Thermal performance. With the miniaturization and high integration of integrated circuits, the thermal conductivity of thin film materials directly affects the thermal noise of the device and affects the speed and reliability of its integrated circuit operation. Therefore, the thermal conductivity measurement of thin film materials is of great significance.
  • a more mature method for measuring the thermal conductivity of a film is Cahill D G. Thermal conductivity measurement from 30 to 750K: the 3 ⁇ method [J]. Review of scientific instruments, 1990, 61 (2): 802-808.), the method is to detect the thermal conductivity of the heater by using a micro-nano film material to conduct a change in the electrical signal of the heater by using a metal layer on the film. This method is capable of measuring a film sample of extremely small size and effectively reducing the measurement error caused by black body radiation, while not directly measuring the temperature change but by measuring the change of the electrical signal converted by the change of the temperature of the material during the heat conduction process. Thermal conductivity of micro/nano film materials.
  • the 3 ⁇ method does not consider the interface thermal resistance of the metal layer and the film to be tested, the anisotropy of the film, and the thickness of the metal strip to have a large influence on the measurement result, and the film may be damaged during the process of photolithography. Defects are generated, which have a greater influence on the scattering of phonons and reduce the thermal conductivity of the material.
  • Perichon et al. proposed a thin film thermal conductivity measurement method based on Raman spectroscopy (Perichon S, Lysenko V, Remaki B, et al. Measurement of porous silicon thermal conductivity by micro-Raman scattering [J].
  • the principle is mainly based on Raman spectroscopy: using a laser beam to illuminate the sample to be tested, causing a local temperature rise of the sample at the irradiation site, the temperature rise and The thermal conductivity of the sample is directly related, and the position of the Raman peak of the sample to be tested corresponds to the temperature of the sample.
  • the method uses an optical method to measure the thermal conductivity of the surface of the film, and the film to be tested does not cause damage. Measurement of film thermal conductivity based on micro-Raman method. Different film materials have to re-calibrate the relationship between the Raman peak displacement and temperature of the film to be tested, and this method can only be used to measure the position and temperature of Raman peak. The thermal conductivity of the film material of the relationship is limited.
  • the present invention can realize the non-destructive and accurate measurement of the thermal conductivity of the film by introducing micro-nano fluorescent particles as a temperature sensor on the surface of the film.
  • the micro-nano fluorescent particle temperature sensor function is realized by spectral analysis technology. Since the micro-nano fluorescent particles have a small particle size (generally 1-10 nm), they can be used for micro-nano scale objects and organisms. Cell temperature measurement, micro-nano fluorescent particles in the measurement due to particle size Small at the same time can be well fitted to the measured object.
  • the interface temperature difference generated by the measurement result is negligible and there is no thermal disturbance to the measured object, so that the accuracy of the measured temperature of the measured object is very high.
  • This method makes up for the 3 ⁇ method. And the lack of Raman spectroscopy can more accurately measure the surface temperature of the film while reducing the influence of the interface temperature difference on the measurement.
  • the object of the present invention is to provide a method for measuring thermal conductivity of a film based on micro-nano fluorescent particles, which is used for solving the interface thermal resistance when measuring the thermal conductivity of a film by the 3 ⁇ method in the prior art.
  • the anisotropy of the film, the influence of the thickness of the metal strip and the damage of the film on the thermal conductivity, and the measurement of the limitation by the micro Raman method are large.
  • the present invention provides a method for measuring thermal conductivity of a film based on micro-nano fluorescent particles, characterized in that the measuring method comprises at least:
  • micro-nano fluorescent particles Providing micro-nano fluorescent particles, heating the micro-nano fluorescent particles, and determining a temperature coefficient by measuring a relationship between a characteristic peak displacement of the micro-nano fluorescent particles PL spectrum and a temperature change;
  • the thermal conductivity of the film is measured in combination with the optical power absorption coefficient of the absorption heat source and the shape characteristic parameter of the film to be tested.
  • the measuring method specifically comprises the following steps:
  • the measuring method specifically includes the following steps:
  • the measuring method specifically comprises the following steps:
  • the micro-nano fluorescent particles are heated by laser heating or atom probe heating.
  • the heat source of absorption is carbon particles, microdroplets, quantum dots or quantum clusters.
  • the diameter of the laser spot is 1/10 to 1/100 of the size of the film to be tested.
  • the film to be tested is placed on the substrate in a floating or non-floating manner.
  • the film to be tested is placed on the substrate in a floating manner, the substrate has a groove, and the film to be tested is suspended on a groove of the substrate.
  • the micro-nano fluorescent particles comprise PbSe, CdSe, CdTe, CdSe/Zns, ZnSe, PbS/CdS, Ag 2 Te, InP/ZnS, ZnCuInS/ZnSe/ZnS, graphene quantum dots or quantum clusters. A combination of one or more.
  • micro-nano fluorescent particle-based film thermal conductivity measuring method of the present invention has the following beneficial effects:
  • micro-nano fluorescent particles are introduced for the first time in the measurement of thermal conductivity of the film, and the micro-nano fluorescent particles are used as the temperature sensor. Because of its small particle size, it can be well attached to the measured object and the interface temperature difference caused by the measurement results. It can be neglected and has no thermal disturbance to the measured object. The measurement result is not, there is no thermal disturbance, and the repeatability is good.
  • the measurement is mainly realized by optical method, which will not cause damage to the sample, and it is not necessary to carry out structural processing on the sample during the measurement to avoid cumbersome sample preparation.
  • the film thermal conductivity measuring system based on micro-nano fluorescent particles has no limitation on the type of film to be measured.
  • the film thermal conductivity measurement system based on micro-nano fluorescent particles reduces the influence of thermal convection on the measurement results.
  • FIG. 1 is a schematic flow chart of a method for measuring thermal conductivity of a film of micro-nano fluorescent particles according to the present invention.
  • FIG. 2 is a schematic view showing the structure of a sample structure module according to an embodiment of the present invention.
  • FIG. 3 is a schematic structural view of a sample structure module according to another embodiment of the present invention.
  • the invention provides a film thermal conductivity measuring method based on micro-nano fluorescent particles, as shown in the flow chart of FIG. 1 , the measuring method comprises at least the following steps:
  • step S1 is performed to provide micro-nano fluorescent particles, the micro-nano fluorescent particles are heated, and the temperature coefficient is determined by measuring the relationship between the characteristic peak displacement of the micro-nano fluorescent particles PL spectrum and the temperature change.
  • the micro-nano fluorescent particles may be placed on the film to be tested for heating, or may be directly placed on the substrate for heating, or may be placed on other suitable supports for heating, and are not limited thereto.
  • this embodiment can avoid damage to the film caused by heating when the film to be tested is thin.
  • the manner of heating the micro-nano fluorescent particles is not limited, and may be laser heating or atomic probe heating, and of course, any other suitable heating method, as long as the micro-nano fluorescent particles can be heated.
  • the atom probe heating is to generate Joule heat by electric heating, and then the heat is transmitted to the micro-nano fluorescent particles by contacting the probe with the micro-nano fluorescent particles to achieve heating.
  • micro-nano fluorescent particles themselves is that the position of the characteristic peak of the PL spectrum (photoluminescence spectrum) of the micro-nano fluorescent particles has a good linear relationship with the temperature, and for example, may be PbSe, CdSe, CdTe, CdSe/ a combination of one or more of Zns, ZnSe, PbS/CdS, Ag 2 Te, InP/ZnS, ZnCuInS/ZnSe/ZnS, or graphene quantum dots or quantum clusters, of course, the micro/nano fluorescent particles of the present invention It can also be a non-quantum dot, and there is no limitation here.
  • micro/nano fluorescent particles of the invention can be well adhered to the object to be measured, the interface temperature difference generated by the measurement result is negligible and there is no thermal disturbance to the measured object, the measurement result is not, no thermal disturbance, and the repeatability is good. .
  • the micro-nano fluorescent particles when used to determine the temperature coefficient of the micro-nano fluorescent particles, may be one, two or more.
  • the micro-nano fluorescent particles are one.
  • the micro-nano fluorescent particles are heated to a specific temperature by a heating module, the PL spectrum of the micro-nano fluorescent particles is measured, and the PL spectrum of the micro-nano fluorescent particles is determined according to the PL spectrum at the temperature and the PL spectrum of the micro-nano fluorescent particles at room temperature.
  • the linear relationship between the displacement of the characteristic peak and the temperature, thereby determining the temperature coefficient ⁇ , ⁇ ⁇ / ⁇ T of the micro-nano fluorescent particles, wherein ⁇ is the displacement change of the characteristic peak of the micro-nano fluorescent particle at two temperatures, ⁇ T is Temperature difference.
  • the micro-nano fluorescent particles can be two.
  • ⁇ is micro
  • the amount of change in the characteristic peak of the nano fluorescent particle with temperature, ⁇ T is the temperature difference.
  • T 2 is the temperature at the position of the micro-nano fluorescent particles 252 on the surface of the film to be tested
  • ⁇ 1 is the position of the characteristic peak of the PL spectrum of the micro-nano fluorescent particles 251 when the position temperature of the micro-nano fluorescent particles 251 on the surface of the film to be tested is T 1
  • ⁇ 2 is the position of the characteristic peak of the PL spectrum of the micro/nano fluorescent particles 252 when the position temperature of the surface micro-nano fluorescent particles 252 of the film 1 to be tested is T 2 . Therefore, the temperature coefficient ⁇ of the micro-nano fluorescent particles 251, 252 can be determined by the temperature and the PL spectrum of the two micro-nano fluorescent particles 251, 252.
  • the main purpose of this step is to determine the temperature coefficient of the micro-nano fluorescent particles.
  • step S2 is performed to place the film to be tested on the substrate, and an absorption heat source and the micro-nano fluorescent particles are placed on the surface of the film to be tested.
  • the film to be tested may be placed on the substrate in a floating or non-floating manner. 2 and 3, the substrate 23 may be a groove substrate, and the film 26 to be tested is suspended on the groove of the substrate 23, so that the film itself can be thermally guided. Rate measurement.
  • the film to be tested can also be directly placed on a planar substrate for measurement of comprehensive effective thermal characteristics.
  • the heat source for absorption may be carbon particles, microdroplets, quantum dots or quantum clusters, etc., and is not limited thereto, as long as it has good thermal contact with the film to be tested and has a known absorption coefficient of optical power. .
  • step S3 the film to be tested is irradiated with a laser, and the relationship slope is determined by measuring the relationship between the characteristic peak displacement of the PL spectrum of the micro/nano fluorescent particles and the change of the laser power.
  • the film to be tested is irradiated with a laser, and heat is absorbed by the absorption heat source to generate heat, so that the position of the micro-nano fluorescent particles on the surface of the film to be tested generates a temperature rise, the power of the incident laser light is changed, and one of the micro-nano fluorescent particles is measured.
  • the amount of change in the displacement of the spectral peak of the spectral spectrum of the nano fluorescent particles is determined.
  • the temperature coefficient ⁇ of the micro-nano fluorescent particles can be measured first, and then the coefficient ⁇ can be obtained.
  • the coefficient ⁇ can be measured first, and then the temperature coefficient ⁇ can be obtained, and the measurement order is not limited here.
  • the diameter of the laser spot is 1/10 to 1/100 of the size of the film to be tested.
  • step S4 is performed to combine the optical power absorption coefficient of the absorption heat source and the shape characteristic parameter of the film to be tested to measure the thermal conductivity of the film.
  • k is the thermal conductivity of the film to be tested
  • ⁇ is the optical power absorption coefficient of the absorption heat source
  • ⁇ P is the incident laser change amount
  • ⁇ P is the power difference absorbed by the film to be tested
  • ⁇ T is the temperature difference
  • w is The width of the film to be tested
  • h is the thickness
  • l is the length of the dangling or the distance between the two micro-nano fluorescent particles.

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Abstract

一种基于微纳荧光颗粒的薄膜热导率测量方法，所述测量方法包括：提供微纳荧光颗粒，加热微纳荧光颗粒，通过测量微纳荧光颗粒PL谱(光致发光光谱)特征峰位移与温度变化的关系，确定温度系数（S1）；将待测薄膜置于衬底上，并在待测薄膜表面放置吸收热源和微纳荧光颗粒（S2）；利用激光照射待测薄膜，通过测量微纳荧光颗粒的PL谱特征峰位移与激光功率变化的关系，确定关系斜率（S3）；最后结合吸收热源的光功率吸收系数以及待测薄膜的形状特征参数，实现薄膜热导率的测量（S4）。利用该测量方法可以实现对微纳米薄膜热导率的无损、便捷、可靠测量。

Description

一种基于微纳荧光颗粒的薄膜热导率测量方法 技术领域
本发明属于微纳米尺度热系数测量领域，特别是涉及一种基于微纳荧光颗粒的薄膜热导率测量方法。
背景技术
在微电子等高科技领域中，薄膜材料在MEMS以及微电子器件设计以及制作过程中不可或缺，而薄膜材料的热导率、比热和热扩散率等热参数性能对决定器件以及集成电路的散热性能。随着集成电路小型化以及高度集成化，薄膜材料的热导率直接影响器件的热噪声进而影响其集成电路运行的速度以及可靠性，因此薄膜材料的热导率测量具有重要意义。
薄膜热导率测量方法中较为成熟的方法为Cahill所发明的3ω法(Cahill D G.Thermal conductivity measurement from 30 to 750K:the 3ω method[J].Review of scientific instruments,1990,61(2):802-808.)，该方法是通过在薄膜上度金属层，利用微/纳米薄膜材料导热引起加热器电信号的变化来检测其热导率。这种方法能够测量尺寸极小的薄膜样品且能有效减小黑体辐射引起的测量误差，同时不直接测量温度变化而是通过测量材料在导热过程中温度的变化转换为的电信号的变化来实现微/纳米薄膜材料的热导率。但是3ω法未考虑金属层与待测膜的界面热阻、膜的各向异性以及金属条形状厚度对测量结果都有较大的影响，同时在光刻金属层过程可能会对膜造成损伤，产生缺陷，对声子的散射影响较大，降低材料的热导率。Perichon等人提出了基于显微拉曼(Raman)光谱的薄膜热导率测量方法(Perichon S,Lysenko V,Remaki B,et al.Measurement of porous silicon thermal conductivity by micro-Raman scattering[J].Journal of Applied Physics,1999,86(8):4700-4702.)，其原理主要基于Raman光谱效即：使用激光束照射被测试样，会在照射处引起试样的局部温升，该温升与试样的热导率直接相关，同时被测试样的Raman谱峰位置与试样的温度有对应关系。该方法采用光学方法测量薄膜表面热导率，对待测薄膜不产生损伤。基于显微Raman法测量薄膜热导率测量不同薄膜材料都得重新标定待测薄的膜Raman谱峰位移量与温度的关系，且该方法只能用于测量拉曼峰位置与温度有着一定规律关系的薄膜材料热导率，局限性较大。
针对现有薄膜热导率测量方法的问题，本发明通过在薄膜表面引入微纳荧光颗粒作为温度传感器，可以实现薄膜热导率无损、精确测量。利用温度与受激的关系发光性能，通过光谱分析技术实现微纳荧光颗粒温度传感器功能，由于微纳荧光颗粒的粒径较小(一般在1-10nm)因此可以用于微纳尺度物体以及生物细胞的温度测量，在测量中微纳荧光颗粒由于粒径 小同时可以很好的贴合在被测物体上对测量结果产生的界面温度差可以忽略不计且对被测物体无热扰动使得被测物体温度测量的结果精度很高，该方法弥补了3ω法以及Raman光谱的不足，能够更加精确测量薄膜表面温度同时降低了测量时的界面温差对结果的影响。
发明内容
鉴于以上所述现有技术的缺点，本发明的目的在于提供一种基于微纳荧光颗粒的薄膜热导率测量方法，用于解决现有技术中3ω法测量薄膜热导率时界面热阻、膜的各向异性以及金属条形状厚度和薄膜损伤等对热导率造成影响以及利用显微Raman法测量局限性大等的问题。
为实现上述目的及其他相关目的，本发明提供一种基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于，所述测量方法至少包括：
提供微纳荧光颗粒，加热所述微纳荧光颗粒，通过测量所述微纳荧光颗粒PL谱特征峰位移与温度变化的关系，确定温度系数；
将待测薄膜置于衬底上，并在所述待测薄膜表面放置吸收热源和所述微纳荧光颗粒；
利用激光照射所述待测薄膜，通过测量所述微纳荧光颗粒的PL谱特征峰位移与激光功率变化的关系，确定关系斜率；
最后结合所述吸收热源的光功率吸收系数以及所述待测薄膜的形状特征参数，实现薄膜热导率的测量。
优选地，所述测量方法具体包括如下步骤：
1-1)提供一衬底，所述衬底上放置悬空宽度为w、厚度为h的待测薄膜，并在所述待测薄膜表面放置一吸收热源和两个距离为l的微纳荧光颗粒；
1-2)利用加热模块加热两个所述微纳荧光颗粒，设定加热模块的温度，测量在不同温度下所述微纳荧光颗粒的PL谱，确定所述微纳荧光颗粒的温度系数χ＝Δλ/ΔT，其中，Δλ为所述微纳荧光颗粒特征峰随温度变化的位移变化量，ΔT为温差值；
1-3)利用激光照射所述待测薄膜，通过所述吸收热源吸收激光能量产生热量，使所述待测薄膜表面所述微纳荧光颗粒位置产生温升，改变入射激光的功率，测量其中一个微纳荧光颗粒的PL光谱特征峰的位移随激光功率变化的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下微纳荧光颗粒PL光谱特征峰的位移变化量；
1-4)最后根据热导率公式k＝(αχ/ω)*(wh/l)-1，获得所述待测薄膜的热导率，α为所述吸收热源的光功率吸收系数。
所述测量方法具体包括如下步骤：
2-1)提供一衬底，所述衬底上放置悬空宽度为w、悬空长度为l、厚度为h的待测薄膜，并在所述待测薄膜表面放置一吸收热源和一微纳荧光颗粒；
2-2)利用加热模块加热所述微纳荧光颗粒至特定温度，测量所述微纳荧光颗粒的PL光谱，根据该温度下的PL光谱和室温下所述微纳荧光颗粒的PL光谱，确定所述微纳荧光颗粒PL光谱特征峰的位移与温度之间的线性关系，从而确定所述微纳荧光颗粒的温度系数χ，χ＝Δλ/ΔT，其中，Δλ为两个温度下所述微纳荧光颗粒特征峰的位移变化量，ΔT为温差值；
2-3)改变入射激光的功率，根据激光功率与所述微纳荧光颗粒PL光谱特征峰的位移的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下所述微纳荧光颗粒PL光谱特征峰的位移变化量；
2-4)最后根据热导率公式k＝(αχ/ω)*(wh/l)-1，获得所述待测薄膜的热导率，α为所述吸收热源的光功率吸收系数。
优选地，所述测量方法具体包括如下步骤：
3-1)提供一衬底，所述衬底上放置悬空宽度为w、厚度为h的待测薄膜，并在所述待测薄膜表面放置一吸收热源和和N个微纳荧光颗粒，其中各个量子点的距离分别为l11，l12，l13……lxy，其中x，y表示第x个微纳荧光颗粒与y微纳荧光颗粒之间的距离，其中x与y都小于N，N＞2。
3-2)利用加热模块加热所述微纳荧光颗粒，设定加热模块的温度，测量在不同温度下微纳荧光颗粒的PL谱，确定微纳荧光颗粒的温度系数χ＝Δλ/ΔT，其中，Δλ为微纳荧光颗粒特征峰随温度变化的位移变化量，ΔT为温差值；
3-3)利用激光照射所述待测薄膜，通过吸收热源吸收激光能量产生热量，使所述待测薄膜表面微纳荧光颗粒位置产生温升，改变入射激光的功率，测量其中一个微纳荧光颗粒的PL光谱特征峰的位移随激光功率变化的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下微纳荧光颗粒PL光谱特征峰的位移变化量；
3-4)最后根据热导率公式kxy＝(αχ/ω)*(wh/lxy)-1，获得待测薄膜的热导率，α为所述吸收热源的光功率吸收系数，其中kxy为第x个微纳荧光颗粒与y微纳荧光颗粒之间的距离范围内的薄膜热导率。
优选地，加热所述微纳荧光颗粒的方式可以为激光加热或者原子探针式加热。
优选地，所述吸收热源为碳颗粒、微液滴、量子点或量子团簇。
优选地，所述激光光斑的直径为所述待测薄膜尺寸的1/10～1/100。
优选地，所述待测薄膜以悬空或者非悬空方式放置在所述衬底上。
优选地，所述待测薄膜若以悬空方式放置在所述衬底上，所述衬底具有凹槽，所述待测薄膜悬空在所述衬底的凹槽上。
优选地，所述微纳荧光颗粒包括PbSe、CdSe、CdTe、CdSe/Zns、ZnSe、PbS/CdS、Ag2Te、InP/ZnS、ZnCuInS/ZnSe/ZnS、石墨烯量子点或量子团簇中的一种或多种的组合。
如上所述，本发明的基于微纳荧光颗粒的薄膜热导率测量方法，具有以下有益效果：
1、在薄膜热导率测量中首次引入微纳荧光颗粒，以微纳荧光颗粒作为温度传感器，由于其粒径小同时可以很好的贴合在被测物体上对测量结果产生的界面温度差可以忽略不计且对被测物体无热扰动对测量结果不、无热扰动，重复性好。
2、测量中主要通过光学方法来实现，不会对样品造成损伤，且在测量时无需对样品进行结构上的加工避免制样上的繁琐。
3、薄膜热导率测量过程中只需一次标定微纳荧光颗粒PL谱峰位移量与温度的关系，且微纳荧光颗粒温度线性关系良好，使在热导率测量过程中温度的确定更为方便、更为精确。
4、基于微纳荧光颗粒的薄膜热导率测量系统对所测量的薄膜种类没有限制。
5、基于微纳荧光颗粒的薄膜热导率测量系统降低热对流对测量结果的影响。
附图说明
图1为本发明微纳荧光颗粒的薄膜热导率测量方法的流程示意图。
图2为本发明一个实施例中样品结构模块的结构示意图。
图3为本发明另一个实施例中样品结构模块的结构示意图。
元件标号说明
23                     衬底
24                     吸收热源
25、251、252           微纳荧光颗粒
26                     待测薄膜
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精 神下进行各种修饰或改变。
请参阅附图。需要说明的是，本实施例中所提供的图示仅以示意方式说明本发明的基本构想，遂图式中仅显示与本发明中有关的组件而非按照实际实施时的组件数目、形状及尺寸绘制，其实际实施时各组件的型态、数量及比例可为一种随意的改变，且其组件布局型态也可能更为复杂。
本发明提供一种基于微纳荧光颗粒的薄膜热导率测量方法，如图1所示流程图，所述测量方法至少包括如下步骤：
首先执行步骤S1，提供微纳荧光颗粒，加热所述微纳荧光颗粒，通过测量所述微纳荧光颗粒PL谱特征峰位移与温度变化的关系，确定温度系数。
所述微纳荧光颗粒可以放置在待测薄膜上加热，也可以直接放置在衬底上加热，也可以放置在其他合适的支撑体上加热，在此不限。当将所述微纳荧光颗粒直接置于衬底表面进行加热测量时，这种实施方式可以避免当待测薄膜较薄时加热对薄膜造成的损伤。
本步骤中，加热所述微纳荧光颗粒的方式不限，可以为激光加热或者原子探针式加热，当然还可以是其他任何合适的加热方式，只要能对所述微纳荧光颗粒加热即可。其中的原子探针式加热是利用电加热产生焦耳热，再通过探针与微纳荧光颗粒接触将热量传导至微纳荧光颗粒，实现加热。
对于所述微纳荧光颗粒本身的要求是，微纳荧光颗粒的PL光谱(光致发光光谱)特征峰的位置与温度需要具有良好的线性关系，例如，可以是PbSe、CdSe、CdTe、CdSe/Zns、ZnSe、PbS/CdS、Ag2Te、InP/ZnS、ZnCuInS/ZnSe/ZnS、或石墨烯量子点或量子团簇中的一种或多种的组合，当然，本发明的微纳荧光颗粒也可以是非量子点，在此不做限制。
本发明的微纳荧光颗粒可以很好的贴合在被测物体上，对测量结果产生的界面温度差可以忽略不计且对被测物体无热扰动对测量结果不、无热扰动，重复性好。
另外，用来确定微纳荧光颗粒温度系数时，微纳荧光颗粒可以是一个、两个或者两个以上。
在一个实施例中，微纳荧光颗粒为一个。利用加热模块加热所述微纳荧光颗粒至特定温度，测量微纳荧光颗粒的PL光谱，根据该温度下的PL光谱和室温下微纳荧光颗粒的PL光谱，确定所述微纳荧光颗粒PL光谱特征峰的位移与温度之间的线性关系，从而确定微纳荧光颗粒的温度系数χ，χ＝Δλ/ΔT，其中，Δλ为两个温度下微纳荧光颗粒特征峰的位移变化量，ΔT为温差值。
具体地，如图3所示，微纳荧光颗粒25在中低温条件下其PL谱特征峰的位移与温度有着很好的线性关系，线性关系可以表示为λ＝χ*T+A，A为常数，χ为温度系数，所以温差值 ΔT＝T1-T2＝(λ1-λ2)/χ＝Δλ/χ，其中T1为待测薄膜26表面微纳荧光颗粒25加热后温度，T2为室温，λ1是待测薄膜表面微纳荧光颗粒25位置温度为T1时微纳荧光颗粒25的PL谱特征峰的位置，λ2是待测薄膜1表面微纳荧光颗粒25在室温T2时的PL谱特征峰的位置。因此，微纳荧光颗粒25的温度系数χ可以通过温度以及微纳荧光颗粒25的PL光谱确定。
在另一个实施例中，微纳荧光颗粒可以是两个。利用加热模块加热两个微纳荧光颗粒，设定加热模块的温度，测量在不同温度下微纳荧光颗粒的PL谱，确定微纳荧光颗粒的温度系数χ＝Δλ/ΔT，其中，Δλ为微纳荧光颗粒特征峰随温度变化的位移变化量，ΔT为温差值。
具体地，如图2所示，微纳荧光颗粒在中低温条件下其PL谱特征峰的位移与温度有着很好的线性关系，线性关系可以表示为λ＝χ*T+A，A为常数，χ为温度系数，所以两处的温差值ΔT＝T1-T2＝(λ1-λ2)/χ＝Δλ/χ，其中T1为待测薄膜26表面微纳荧光颗粒251位置的温度，T2为待测薄膜表面微纳荧光颗粒252位置的温度，λ1是待测薄膜表面微纳荧光颗粒251位置温度为T1时微纳荧光颗粒251的PL谱特征峰的位置，λ2是待测薄膜1表面微纳荧光颗粒252位置温度为T2时微纳荧光颗粒252的PL谱特征峰的位置。因此，微纳荧光颗粒251、252的温度系数χ可以通过温度以及两处微纳荧光颗粒251、252的PL光谱确定。
在又一实施例中，微纳荧光颗粒可以是两个以上，即多个。利用加热模块加热所述微纳荧光颗粒，设定加热模块的温度，测量在不同温度下微纳荧光颗粒的PL谱，确定微纳荧光颗粒的温度系数χ＝Δλ/ΔT，其中，Δλ为微纳荧光颗粒特征峰随温度变化的位移变化量，ΔT为温差值。
本步骤的主要目的就是确定微纳荧光颗粒的温度系数。
然后执行步骤S2，将待测薄膜置于衬底上，并在所述待测薄膜表面放置吸收热源和所述微纳荧光颗粒。
所述待测薄膜可以以悬空或者非悬空方式放置在所述衬底上。如图2和3所示衬底，所述衬底23可以是凹槽衬底，则所述待测薄膜26悬空在所述衬底23的凹槽上，这样可以对待测薄膜本身进行热导率测量。所述待测薄膜也可以直接放置在平面衬底上，进行综合有效热特性的测量。
所述吸收热源可以为碳颗粒、微液滴、量子点或量子团簇等等，在此不限，只要与待测薄膜有很好的热接触并且具有已知的光功率吸收系数的都行。
接着执行步骤S3，利用激光照射所述待测薄膜，通过测量所述微纳荧光颗粒的PL谱特征峰位移与激光功率变化的关系，确定关系斜率。
具体地，利用激光照射所述待测薄膜，通过吸收热源吸收激光能量产生热量，使所述待测薄膜表面微纳荧光颗粒位置产生温升，改变入射激光的功率，测量其中一个微纳荧光颗粒 的PL光谱特征峰的位移随激光功率变化的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下微纳荧光颗粒PL光谱特征峰的位移变化量。
需要说明的是，既可以先测量获得微纳荧光颗粒的温度系数χ，再测量获得系数ω；也可以先测量获得系数ω，再测量获得温度系数χ，在此不限制测量顺序。
在本步骤中，优选地，所述激光光斑的直径为所述待测薄膜尺寸的1/10～1/100。
最后执行步骤S4，结合所述吸收热源的光功率吸收系数以及所述待测薄膜的形状特征参数，实现薄膜热导率的测量。
本步骤中，根据热导率公式k＝(αχ/ω)*(wh/l)-1，获得待测薄膜的热导率，α为所述吸收热源的光功率吸收系数。
具体推导如下：
从待测薄膜的热导G定义式出发，其公式推导如下：
G＝k*wh/l＝αΔP/ΔT，由此，
k＝(αΔP/ΔT)/(wh/l)
其中，上式中k为待测薄膜的热导率，α是吸收热源的光功率吸收系数，ΔP是入射激光变化量，αΔP为待测薄膜吸收的功率差值，ΔT为温差值，w为待测薄膜悬空宽度，h为厚度，l为悬空长度或者两处微纳荧光颗粒之间的距离。当微纳荧光颗粒为多个时，公式中的l为lxy，表示第x个微纳荧光颗粒与y微纳荧光颗粒之间的距离，测出来的热导率k则为第x个微纳荧光颗粒与y微纳荧光颗粒之间的距离范围内的薄膜热导率。
将ΔT＝T1-T2＝(λ1-λ2)/χ＝Δλ/χ代入上式可以得到：k＝χ*(Δλ/αΔP)-1/(wh/l)，在该公式中含有Δλ/ΔP，由于在同一环境温度条件下薄膜材料的热导G＝αΔP/ΔT基本不发生改变，所以吸收功率差值αΔP与温差ΔT的比值是不变的，由ΔT＝Δλ/χ可以推出αΔP与Δλ也是线性关系。因此，通过改变入射激光的功率P，再测量待测薄膜表面微纳荧光颗粒的PL谱特征位移关系可以确定Δλ/ΔP的关系斜率值ω，最后，其热导率公式简化为：k＝αχ/ω*(wh/l)-1，其中的χ和ω值由步骤S1和S3的方法来测量确定，α是已知常数。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (10)

  1. 一种基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于，所述测量方法至少包括：
    提供微纳荧光颗粒，加热所述微纳荧光颗粒，通过测量所述微纳荧光颗粒PL谱特征峰位移与温度变化的关系，确定温度系数；
    将待测薄膜置于衬底上，并在所述待测薄膜表面放置吸收热源和所述微纳荧光颗粒；
    利用激光照射所述待测薄膜，通过测量所述微纳荧光颗粒的PL谱特征峰位移与激光功率变化的关系，确定关系斜率；
    最后结合所述吸收热源的光功率吸收系数以及所述待测薄膜的形状特征参数，实现薄膜热导率的测量。
  2. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述测量方法具体包括如下步骤：
    1-1)提供一衬底，所述衬底上放置悬空宽度为w、厚度为h的待测薄膜，并在所述待测薄膜表面放置一吸收热源和两个距离为l的微纳荧光颗粒；
    1-2)利用加热模块加热两个所述微纳荧光颗粒，设定加热模块的温度，测量在不同温度下所述微纳荧光颗粒的PL谱，确定所述微纳荧光颗粒的温度系数χ＝Δλ/ΔT，其中，Δλ为所述微纳荧光颗粒特征峰随温度变化的位移变化量，ΔT为温差值；
    1-3)利用激光照射所述待测薄膜，通过所述吸收热源吸收激光能量产生热量，使所述待测薄膜表面所述微纳荧光颗粒位置产生温升，改变入射激光的功率，测量其中一个微纳荧光颗粒的PL光谱特征峰的位移随激光功率变化的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下微纳荧光颗粒PL光谱特征峰的位移变化量；
    1-4)最后根据热导率公式k＝(αχ/ω)*(wh/l)-1，获得所述待测薄膜的热导率，α为所述吸收热源的光功率吸收系数。
  3. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述测量方法具体包括如下步骤：
    2-1)提供一衬底，所述衬底上放置悬空宽度为w、悬空长度为l、厚度为h的待测薄膜，并在所述待测薄膜表面放置一吸收热源和一微纳荧光颗粒；
    2-2)利用加热模块加热所述微纳荧光颗粒至特定温度，测量所述微纳荧光颗粒的PL光谱，根据该温度下的PL光谱和室温下所述微纳荧光颗粒的PL光谱，确定所述微纳荧 光颗粒PL光谱特征峰的位移与温度之间的线性关系，从而确定所述微纳荧光颗粒的温度系数χ，χ＝Δλ/ΔT，其中，Δλ为两个温度下所述微纳荧光颗粒特征峰的位移变化量，ΔT为温差值；
    2-3)改变入射激光的功率，根据激光功率与所述微纳荧光颗粒PL光谱特征峰的位移的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下所述微纳荧光颗粒PL光谱特征峰的位移变化量；
    2-4)最后根据热导率公式k＝(αχ/ω)*(wh/l)-1，获得所述待测薄膜的热导率，α为所述吸收热源的光功率吸收系数。
  4. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述测量方法具体包括如下步骤：
    3-1)提供一衬底，所述衬底上放置悬空宽度为w、厚度为h的待测薄膜，并在所述待测薄膜表面放置一吸收热源和N个微纳荧光颗粒，其中各个微纳荧光颗粒的距离分别为l11，l12，l13……lxy，其中x，y表示第x个微纳荧光颗粒与第y个微纳荧光颗粒之间的距离，x与y都小于N，N＞2；
    3-2)利用加热模块加热所述微纳荧光颗粒，设定加热模块的温度，测量在不同温度下所述微纳荧光颗粒的PL谱，确定所述微纳荧光颗粒的温度系数χ＝Δλ/ΔT，其中，Δλ为所述微纳荧光颗粒特征峰随温度变化的位移变化量，ΔT为温差值；
    3-3)利用激光照射所述待测薄膜，通过所述吸收热源吸收激光能量产生热量，使所述待测薄膜表面所述微纳荧光颗粒位置产生温升，改变入射激光的功率，测量其中一个微纳荧光颗粒的PL光谱特征峰的位移随激光功率变化的线性关系，确定两者之间的关系斜率ω，ω＝Δλ/ΔP，其中，ΔP为入射激光功率的变化量，Δλ为不同入射激光功率下微纳荧光颗粒PL光谱特征峰的位移变化量；
    3-4)最后根据热导率公式kxy＝(αχ/ω)*(wh/lxy)-1，获得所述待测薄膜的热导率，α为所述吸收热源的光功率吸收系数，其中kxy为第x个微纳荧光颗粒与第y个微纳荧光颗粒之间的距离范围内的薄膜热导率。
  5. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：加热所述微纳荧光颗粒的方式可以为激光加热或者原子探针式加热。
  6. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述吸收 热源为碳颗粒、微液滴、量子点或量子团簇。
  7. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述激光光斑的直径为所述待测薄膜尺寸的1/10～1/100。
  8. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述待测薄膜以悬空或者非悬空方式放置在所述衬底上。
  9. 根据权利要求8所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述待测薄膜若以悬空方式放置在所述衬底上，所述衬底具有凹槽，所述待测薄膜悬空在所述衬底的凹槽上。
  10. 根据权利要求1所述的基于微纳荧光颗粒的薄膜热导率测量方法，其特征在于：所述微纳荧光颗粒包括PbSe、CdSe、CdTe、CdSe/Zns、ZnSe、PbS/CdS、Ag2Te、InP/ZnS、ZnCuInS/ZnSe/ZnS、石墨烯量子点或量子团簇中的一种或多种的组合。
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CN107843616B (zh) * 2017-11-15 2020-05-22 宁波星河材料科技有限公司 快速测量薄膜材料的热导率的装置和方法
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