CN106970060B - Measurement method of long phosphorescence spectrum induced by femtosecond laser micromachining system - Google Patents
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- 238000001296 phosphorescence spectrum Methods 0.000 title claims abstract description 23
- 238000005459 micromachining Methods 0.000 title claims abstract description 19
- 238000000691 measurement method Methods 0.000 title abstract description 7
- 238000001228 spectrum Methods 0.000 claims abstract description 21
- 230000003595 spectral effect Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000013307 optical fiber Substances 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000036962 time dependent Effects 0.000 claims 1
- 238000004020 luminiscence type Methods 0.000 abstract description 11
- 230000007246 mechanism Effects 0.000 abstract description 8
- 230000005284 excitation Effects 0.000 abstract description 2
- 230000006698 induction Effects 0.000 abstract 2
- 238000002381 microspectrum Methods 0.000 abstract 1
- 230000001939 inductive effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- -1 rare earth ions Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 235000012215 calcium aluminium silicate Nutrition 0.000 description 1
- 239000000404 calcium aluminium silicate Substances 0.000 description 1
- WNCYAPRTYDMSFP-UHFFFAOYSA-N calcium aluminosilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O WNCYAPRTYDMSFP-UHFFFAOYSA-N 0.000 description 1
- 229940078583 calcium aluminosilicate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G01N21/6408—Fluorescence; Phosphorescence with measurement of decay time, time resolved fluorescence
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Abstract
Description
技术领域technical field
本发明属于光谱测量技术领域，是一种利用飞秒激光微加工系统诱导长磷光光谱的测量方法。The invention belongs to the technical field of spectrum measurement, and relates to a measurement method for inducing long phosphorescence spectrum by using a femtosecond laser micromachining system.
背景技术Background technique
长磷光是指当激发光源切断后能持续发光的现象。传统的长磷光材料，又名“夜光粉”，在日光或者紫外光的短暂照射下，撤去光源，仍在很长一段时间内持续发光。传统的长磷光材料已经在隐蔽照明、紧急照明设施，航空、航海和汽车仪表盘显示以及道路标记等领域得到了广泛应用。Long phosphorescence refers to the phenomenon of continuous light emission after the excitation light source is turned off. Traditional long-phosphorescent materials, also known as "luminous powder", continue to emit light for a long period of time when the light source is removed under the short-term exposure of sunlight or ultraviolet light. Traditional long phosphorescent materials have been widely used in concealed lighting, emergency lighting installations, aviation, marine and automotive dashboard displays, and road markings.
1998年，邱建荣小组发现，飞秒激光辐照含稀土离子(Ce3+、Tb3+、Pr3+)的钙铝硅玻璃，撤去激光后，被飞秒激光作用的部分还发出明亮的磷光。这种激光诱导长磷光现象引起了国内外的重视。后来他们又系统报道了稀土离子(Eu2+)、过渡金属离子(Mn2+)掺杂的硼酸盐以及掺锗的石英玻璃等在飞秒激光辐照后的长磷光现象。In 1998, Qiu Jianrong's group discovered that calcium-aluminosilicate glass containing rare earth ions (Ce 3+ , Tb 3+ , Pr 3+ ) was irradiated by femtosecond laser. After the laser was removed, the part affected by the femtosecond laser also emitted bright phosphorescence. . This laser-induced long phosphorescence phenomenon has attracted much attention at home and abroad. Later, they systematically reported the long phosphorescence phenomena of rare earth ions (Eu 2+ ), transition metal ions (Mn 2+ ) doped borates and germanium doped quartz glass after femtosecond laser irradiation.
以一玻璃块体的长磷光样品为例，经紫外光照射，样品的表面和内部的所有区域都发出长磷光。而飞秒激光经过物镜的聚焦，可以在样品表面以及内部的任意深度加工出任意尺寸的图形(最小可达微米量级)，加工出的图形区域就是长磷光发光区。所以说，飞秒激光诱导的长磷光是空间选择性的。这种空间可选择性的长磷光在三维立体显示、三维光学存储以及工艺美术上有重要应用。Taking a long phosphorescent sample of a glass block as an example, when irradiated with ultraviolet light, all areas of the surface and interior of the sample emit long phosphorescence. After the femtosecond laser is focused by the objective lens, it can process patterns of any size (the smallest can reach the order of micrometers) on the surface of the sample and at any depth in the interior. The processed pattern area is the long phosphorescent light-emitting area. Therefore, femtosecond laser-induced long phosphorescence is spatially selective. This spatially selective long phosphorescence has important applications in 3D stereoscopic display, 3D optical storage and arts and crafts.
为了研究飞秒激光诱导的长磷光的发光机理与发光性能，就必须精确测量出长磷光光谱以及光谱随时间的变化。然而，飞秒激光诱导的长磷光的发光特点是，激光先加工的区域先发光，后作用的区域后发光。比如说，我们用激光扫出一个1mm×1mm的区域来测光谱，当激光扫完这个1mm2的区域的最后一个点时，激光扫的第一个点的长磷光已经发光一段时间了。有的长磷光材料会有多个发光中心，不仅光谱强度随时间衰减，光谱的谱型也会随着时间变化。光谱的精确测量就要求飞秒激光作用的区域一起发光。然而这种激光作用区域不同步发光的特性就给光谱的精确测量带来了不便。经过实验论证，飞秒激光诱导的长磷光与环境温度有关，当环境温度为0℃时，即使是激光作用过的区域也没有发光现象，然而当环境温度升至室温时，激光作用过的区域会出现长磷光。因此，利用长磷光与温度的关系，开展飞秒激光诱导的长磷光相关机理与性能的研究，就需要一个专门的利用飞秒激光微加工装置诱导长磷光光谱的测量方法。In order to study the luminescence mechanism and luminescence properties of femtosecond laser-induced long phosphorescence, it is necessary to accurately measure the long phosphorescence spectrum and the change of the spectrum with time. However, the luminescence characteristic of femtosecond laser-induced long phosphorescence is that the region processed first by the laser emits light first, and the region that is acted on later emits light later. For example, we use the laser to scan a 1mm×1mm area to measure the spectrum. When the laser scans the last point of this 1mm2 area, the long phosphorescence of the first point of the laser scan has been emitting for a period of time. Some long phosphorescent materials have multiple luminescent centers, not only the spectral intensity decays with time, but also the spectral type of the spectrum. Accurate measurement of the spectrum requires the femtosecond laser to emit light together. However, the characteristic of the asynchronous emission of the laser action area brings inconvenience to the accurate measurement of the spectrum. After experimental demonstration, the long phosphorescence induced by femtosecond laser is related to the ambient temperature. When the ambient temperature is 0 °C, there is no luminescence even in the laser-acted area. However, when the ambient temperature rises to room temperature, the laser-acted area does not emit light. Long phosphorescence occurs. Therefore, using the relationship between long phosphorescence and temperature to carry out research on the mechanism and performance of femtosecond laser-induced long phosphorescence requires a special measurement method for long phosphorescence spectra induced by femtosecond laser micromachining devices.
发明内容SUMMARY OF THE INVENTION
本发明目的在于解决飞秒激光诱导的长磷光光谱不能精确测量的问题，利用飞秒激光诱导的长磷光与温度的关系，提出一种利用飞秒激光微加工装置诱导长磷光光谱的测量方法。该方法结构简单，操作安全方便，可以测量不同温度以及不同时刻的长磷光光谱，然后用作图软件计算出某一温度下每个时刻对应的光谱积分强度，得到不同温度下光谱积分强度随时间衰减图，并作非线性拟合，根据拟合的参数，研究飞秒激光诱导的长磷光的发光机理。The purpose of the invention is to solve the problem that the long phosphorescence spectrum induced by femtosecond laser cannot be accurately measured, and a method for measuring the long phosphorescence spectrum induced by a femtosecond laser micromachining device is proposed by utilizing the relationship between the long phosphorescence induced by the femtosecond laser and the temperature. The method is simple in structure, safe and convenient in operation, can measure long phosphorescence spectra at different temperatures and at different times, and then use it as a graph software to calculate the spectral integral intensity corresponding to each time at a certain temperature, and obtain the spectral integral intensity at different temperatures with time. According to the fitted parameters, the luminescence mechanism of femtosecond laser-induced long phosphorescence was studied.
本发明的技术解决方案如下：The technical solution of the present invention is as follows:
利用飞秒激光微加工装置诱导长磷光光谱的测量方法，包括飞秒激光微加工装置，其特征在于，该系统还包括：显微光谱收集装置及温控装置；A method for measuring long phosphorescence spectrum induced by a femtosecond laser micromachining device, including a femtosecond laser micromachining device, characterized in that the system further includes: a microspectroscope collection device and a temperature control device;
所述的飞秒激光微加工装置，包括飞秒激光器，反射飞秒激光的二向色镜，聚焦飞秒激光的显微物镜，反射光谱的反射镜，三位可移动的载物台以及放于样品台上的样品。从飞秒激光器出射的飞秒激光通过显微物镜，聚焦到样品内部，实现对样品内部的精确加工。The femtosecond laser micromachining device includes a femtosecond laser, a dichroic mirror that reflects the femtosecond laser, a microscope objective lens that focuses the femtosecond laser, a reflector that reflects the spectrum, a three-position movable stage, and a sample on the sample stage. The femtosecond laser emitted from the femtosecond laser passes through the microscope objective and is focused into the inside of the sample to achieve precise processing of the inside of the sample.
所述的显微光谱收集装置包括两个微透镜，光纤以及光谱仪。飞秒激光诱导的长磷光光谱被显微物镜收集，透过二向色镜，然后被反射镜反射进入微透镜聚焦，耦合到光纤中，再通过另一个微透镜导入到光谱仪狭缝中。The microscopic spectrum collection device includes two microlenses, an optical fiber and a spectrometer. The femtosecond laser-induced long phosphorescence spectrum is collected by the microscope objective, transmitted through the dichroic mirror, and then reflected by the mirror into the microlens focused, coupled into the fiber, and then directed into the spectrometer slit through another microlens.
所述的温控装置包括容器，放置在该容器内的样品台、蒸馏水以及可调节温度的智能加热棒。样品放在样品台上，蒸馏水淹没样品。飞秒激光加工时，使水温为0℃，所以飞秒激光加工过程中，被作用的区域不发光，待激光加工结束后，使水温加热到室温，此时飞秒激光加工的区域同时发光，用光谱收集装置可精确测量出长磷光的光谱强度及谱型随时间的变化，然后对采集的光谱进行强度积分，得到光谱积分强度随时间衰减图，并作非线性拟合，根据拟合的参数，研究飞秒激光诱导的长磷光的发光机理。The temperature control device includes a container, a sample stage placed in the container, distilled water and an intelligent heating rod with adjustable temperature. The sample is placed on the sample stage and the sample is submerged in distilled water. During femtosecond laser processing, the water temperature is set to 0 °C, so during the femtosecond laser processing, the affected area does not emit light. After the laser processing is completed, the water temperature is heated to room temperature. At this time, the area processed by the femtosecond laser emits light at the same time. The spectral intensity and spectral type of long phosphorescence can be accurately measured with the spectral collection device, and then the intensity of the collected spectrum can be integrated to obtain a graph of the spectral integrated intensity decay with time. parameters to study the luminescence mechanism of femtosecond laser-induced long phosphorescence.
与现有技术相比，本发明的技术效果如下：Compared with the prior art, the technical effect of the present invention is as follows:
本发明利用飞秒激光诱导的长磷光与温度的关系，将样品置于温控装置中，通过调节温度使飞秒激光作用的区域一起发光，能够精确地测量出长磷光光谱其强度及谱型随时间的变化。此外，通过调节到不同温度，可以对比不同温度下长磷光光谱随时间的衰减，这对于研究飞秒激光诱导的长磷光的发光机理及发光特性具有重要意义。The invention utilizes the relationship between the long phosphorescence induced by the femtosecond laser and the temperature, places the sample in a temperature control device, and adjusts the temperature to make the area acted by the femtosecond laser emit light together, so that the intensity and spectral type of the long phosphorescence spectrum can be accurately measured. change over time. In addition, by adjusting to different temperatures, the decay of long phosphorescence spectra at different temperatures can be compared with time, which is of great significance for studying the luminescence mechanism and luminescence properties of femtosecond laser-induced long phosphorescence.
本发明结构简单、操作方便，性能稳定，给精确测量飞秒激光诱导的长磷光光谱提供了可靠高效的途径。The invention has the advantages of simple structure, convenient operation and stable performance, and provides a reliable and efficient way to accurately measure the long phosphorescence spectrum induced by the femtosecond laser.
附图说明Description of drawings
图1是利用飞秒激光微加工装置诱导长磷光光谱的测量方法示意图Fig. 1 is the schematic diagram of the measurement method of induced long phosphorescence spectrum using femtosecond laser micromachining device
具体实施方式Detailed ways
下面结合附图和实施例对本发明做进一步说明，但不应因此限制本发明的保护范围。The present invention will be further described below with reference to the accompanying drawings and embodiments, but the protection scope of the present invention should not be limited accordingly.
请参阅图1，图1是利用飞秒激光微加工装置诱导长磷光光谱的测量方法示意图，如图所示，本发明是一种利用飞秒激光微加工装置诱导长磷光光谱的测量方法，包括飞秒激光微加工装置，其特征在于，该系统还包括：显微光谱收集装置及温控装置；Please refer to FIG. 1. FIG. 1 is a schematic diagram of a measurement method for inducing long phosphorescence spectrum using a femtosecond laser micromachining device. As shown in the figure, the present invention is a measurement method for inducing long phosphorescence spectrum using a femtosecond laser micromachining device, including The femtosecond laser micromachining device is characterized in that the system further comprises: a microscopic spectrum collection device and a temperature control device;
所述的飞秒激光微加工装置包括飞秒激光器1，反射飞秒激光的二向色镜3，聚焦飞秒激光的显微物镜4，反射长磷光光谱的反射镜12，三位可移动的载物台5以及放于样品台上的样品6。The femtosecond laser micromachining device includes a femtosecond laser 1, a dichroic mirror 3 for reflecting the femtosecond laser, a microscope objective lens 4 for focusing the femtosecond laser, a reflecting mirror 12 for reflecting the long phosphorescence spectrum, and a three-position movable mirror. Stage 5 and sample 6 placed on the sample stage.
所述的显微光谱收集装置包括微透镜13、光纤14、微透镜15以及光谱仪16；The microscopic spectrum collection device includes a microlens 13, an optical fiber 14, a microlens 15 and a spectrometer 16;
所述的温控装置包括容器9，放置在该容器内的样品台7、蒸馏水8以及可调节温度的智能加热棒10；The temperature control device includes a container 9, a sample stage 7 placed in the container, distilled water 8 and an intelligent heating rod 10 with an adjustable temperature;
从飞秒激光器1出射的飞秒激光2通过二向色镜3反射到显微物镜4中，经物镜4聚焦到样品6内部。样品6放在固定在容器9中的样品台7上，蒸馏水8淹没样品6，此时调节水温为0℃。容器9放在载物台5上，飞秒激光加工过程中，载物台5三维移动，实现对样品的精密加工，被激光加工的区域在0℃下不发光。加工结束后，将水温加热至室温，此时样品被加工的区域同时发出长磷光11，被显微物镜4收集，透过二项色镜3，被反射镜12反射进入第一微透镜13，然后聚焦耦合到光纤14中，再通过第二微透镜15导入到光谱仪16中，测量出室温下的光谱。此后每隔n(n可以任意设置)分钟采集一次长磷光光谱，直到光谱不被探测到。然后用作图软件计算出每个时刻对应的光谱积分强度，得到光谱积分强度随时间衰减图，并作非线性拟合，根据拟合的参数，研究飞秒激光诱导的长磷光的发光机理。The femtosecond laser light 2 emitted from the femtosecond laser 1 is reflected into the microscope objective lens 4 through the dichroic mirror 3 , and is focused into the inside of the sample 6 through the objective lens 4 . The sample 6 is placed on the sample stage 7 fixed in the container 9, and the sample 6 is submerged in the distilled water 8. At this time, the water temperature is adjusted to 0°C. The container 9 is placed on the stage 5. During the femtosecond laser processing, the stage 5 moves three-dimensionally to achieve precise processing of the sample, and the laser-processed area does not emit light at 0°C. After processing, the water temperature is heated to room temperature. At this time, the processed area of the sample emits long phosphorescence 11 at the same time, which is collected by the microscope objective lens 4, passes through the dichroic mirror 3, and is reflected by the reflecting mirror 12 into the first microlens 13. Then, it is focused and coupled into the optical fiber 14, and then introduced into the spectrometer 16 through the second microlens 15, and the spectrum at room temperature is measured. Thereafter, long phosphorescence spectra are collected every n (n can be set arbitrarily) minutes until the spectra are not detected. Then use the graph software to calculate the spectral integral intensity corresponding to each moment, obtain the spectral integral intensity decay graph with time, and make a nonlinear fitting. According to the fitted parameters, the luminescence mechanism of femtosecond laser-induced long phosphorescence is studied.
此外，飞秒激光加工后，可将水温升至任意温度，就可以测量该温度下的长磷光光谱随时间的变化，通过数据处理得到该温度下光谱积分强度随时间衰减曲线，这对长磷光的发光机理和使用性能的研究有重要作用。In addition, after femtosecond laser processing, the water temperature can be raised to any temperature, the change of the long phosphorescence spectrum at this temperature with time can be measured, and the decay curve of the integrated spectral intensity with time at this temperature can be obtained through data processing. The research on the luminescence mechanism and performance of phosphorescence plays an important role.
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