CN105911034A - Mobile platform-based luminescent material performance testing apparatus - Google Patents

Abstract

The utility model relates to a performance test device for luminescent materials based on a mobile platform, which relates to the performance test of luminescent materials. Including an excitation light source, a spectrometer and an integrating sphere, the integrating sphere is provided with a sample stage and a mobile platform, the sample stage is used to place the sample to be tested, and the mobile platform can drive the sample stage to move; the mobile based The luminescent material performance testing device of the platform also includes a microscope and a controller; an opening is provided on the integrating sphere, and when working, the objective lens of the microscope extends into the inside of the integrating sphere through the opening for observation and placement The sample to be measured in the integrating sphere; the controller is electrically connected with the excitation light source, mobile platform, spectrometer and microscope respectively, and is used to control the actions of the excitation light source, mobile platform, spectrometer and microscope. It can realize the test of the luminescence performance of a single particle phosphor.

Description

Luminescent material performance test device based on mobile platform

technical field

The invention relates to performance testing of luminescent materials, in particular to a performance testing device for luminescent materials based on a mobile platform.

Background technique

Luminescent materials are a class of materials that can realize light conversion, and can be divided into organic luminescent materials and inorganic luminescent materials. Among them, most of the inorganic luminescent materials (excluding quantum dot luminescent materials) are in powder form and are composed of individual solid luminescent particles. The size of any dimension of these particles ranges from tens of nanometers to tens of microns (Vinay Kumar, Shreyas S.Pitale, Varun Mishra, I.M.Nagpure, M.M.Biggs, O.M.Ntwaeaborwa and H.C.Swart.Journal of Alloys and Compounds, 492(2010), L8- L12; Zhen Song, Jing Liao, Xianlin Ding, Xiaolang Liu and Quanlin Liu. Synthesis of YAG phosphor particles with excellent morphology by solidstate reaction, Journal of Crystal Growth, 365(2013), 24-28).

The performance of the luminescent material can be specifically understood through the measurement of the relevant luminescent properties. The measurement of the luminescence properties of traditional phosphors is achieved by measuring the luminescence of phosphors with a macroscopic volume (accumulation of a large number of luminescent particles) (Chinese Patent Publication No.: CN103323438A). For example, the macro-volume phosphor is placed in the sample chamber of the spectrometer, and by setting the instrument parameters, the light of a specific wavelength emitted by the light source irradiates the surface of the phosphor, and the phosphor emits light under the excitation of the light, and the emitted light passes through the detector of the spectrometer Collection and data processing, testing out the photoluminescent performance of the phosphor. Of course, by heating the macro-volume phosphor or putting it into an integrating sphere, the change of the luminescent properties of the macro-volume phosphor with temperature (thermal quenching) and quantum efficiency can be measured.

Since the traditional luminescent material measurement technology is to measure the luminescence of macroscopic volume phosphors, the measurement data is actually based on the statistical results of the luminescence behavior of a large number of luminescent particles. Behavior is unclear; especially when the phosphor is composed of many different luminescent substances (Kang Sik Choi, Soon Duk Jee, Jung Pyo Lee and Chang Hae Kim. Journal of Nanoscience and Nanotechnology, 13(2013), 1867-1870) The luminescent properties measured by traditional luminescent material measurement techniques are a combination of the luminescent properties of a variety of different luminescent substances, and the luminescent properties of each luminescent material cannot be directly determined.

Contents of the invention

The purpose of the present invention is to provide a mobile platform-based luminescent material performance testing device that can directly measure the luminescence properties such as photoluminescent properties, thermal quenching properties and quantum efficiency of a single solid powder particle.

The present invention includes an excitation light source, a spectrometer, an integrating sphere, a microscope and a controller; a sample stage and a moving platform are arranged inside the integrating sphere, the sample stage is used to place the sample to be tested, and the moving platform is used to drive the sample platform to move;

The integrating sphere is provided with an opening, and during operation, the objective lens of the microscope extends into the integrating sphere through the opening for observing the sample to be measured placed in the integrating sphere;

The controller is electrically connected with the excitation light source, the mobile platform, the spectrometer and the microscope respectively, and is used to control the actions of the excitation light source, the mobile platform, the spectrometer and the microscope.

The microscope can be a stereomicroscope, which can distinguish particles with a size not smaller than 100 nm in any dimension.

The mobile platform can be an omnidirectional mobile platform, which can drive the sample stage to move in all directions.

The omnidirectional mobile platform includes a first electric control platform, a second electric control platform and a third electric control platform;

The first electric control platform can drive the sample stage to rotate 360° around its central axis, the second electric control platform can drive the sample stage to move horizontally along the X-Y direction, and the third electric control platform can drive the sample stage Move vertically along the Z axis.

The minimum rotation angle of the first electronically controlled platform may be less than or equal to 0.5°, and the minimum moving distances of the second electronically controlled platform and the third electrically controlled platform may be less than or equal to 1 μm.

A sealing assembly is provided at the opening, and when the objective lens of the microscope extends into the integrating sphere, the sealing assembly seals the gap between the objective lens and the integrating sphere.

A heating device may be provided inside the integrating sphere, the heating device is electrically connected to the controller, and the heating device is used to heat the sample to be tested on the sample stage.

An auxiliary light source may be provided inside the integrating sphere, and the auxiliary light source is electrically connected to the controller.

The present invention may also include a first guiding fiber, a second guiding fiber and a third guiding fiber;

An optical fiber fixing device may also be provided inside the integrating sphere; one end of the first guiding fiber is connected to the fiber fixing device, the other end of the first guiding fiber is connected to a spectrometer, one end of the second guiding fiber is connected to the fiber fixing device, and the second guiding fiber is connected to the fiber fixing device. The other end of the second conductive fiber is connected to the excitation light source;

A light baffle may be provided on the inner wall of the integrating sphere, one end of the third guiding fiber is connected to the light baffle, and the other end of the third guiding fiber is connected to the spectrometer.

The optical fiber fixing device may be provided with a position sensor, and the position sensor is electrically connected to the controller.

The present invention has following beneficial effect:

The present invention is equipped with a microscope and a mobile platform. When testing, the sample to be tested in the integrating sphere can be observed through the microscope, and the sample to be tested can be moved through the mobile platform, so that the solid powder particles at a certain position can be targeted. Carry out a test to realize the test of the luminescence performance of a single particle phosphor. For phosphor solid powder particles composed of a variety of different substances, the luminescence properties of each phosphor solid powder particle can be directly measured; meanwhile, the present invention has complete functions. Not only can the photoluminescent properties of a single solid powder particle be tested, but also the change of the luminescent property of a single solid powder particle with temperature and the quantum efficiency of a single solid powder particle can be tested.

Description of drawings

Fig. 1 is the structural composition schematic diagram of the embodiment of the present invention;

Fig. 2 is the photoluminescence spectrum of a certain phosphor particle in embodiment 1;

Fig. 3 is the quantum efficiency collection of illustrative plates of certain phosphor particle in embodiment 2;

FIG. 4 is a thermal quenching spectrum diagram of a phosphor particle in Example 3. FIG.

detailed description

In order to make the object, technical solution and advantages of the present invention clearer, the following embodiments will further illustrate the present invention in conjunction with the accompanying drawings. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.

The embodiment of the present invention is mainly used for testing the luminescent properties of solid powder particles, especially suitable for the luminescent properties of solid powder particles with a particle size greater than or equal to 100 nm. As shown in Figure 1, the embodiment of the present invention includes an excitation light source 05, a spectrometer 03 and an integrating sphere 16. As a possible implementation mode, the excitation light source 05 can be a xenon lamp, a laser or an LED light source; the measurement wavelength range of the spectrometer 03 is greater than or equal to 200nm , less than or equal to 1500nm.

Wherein, the integrating sphere 16 is provided with a sample stage 11 and a mobile platform inside, the sample stage 11 is used to place the sample to be tested, and the mobile platform can drive the sample stage 11 to move. As a possible embodiment, the mobile platform is horizontally arranged on the integrating sphere 16 Inside, and located below the sample stage 11. Preferably, the sample stage 11 is provided with a groove for containing the sample to be tested.

The present invention also includes a microscope 07 and a controller 01. An opening is provided on the integrating sphere 16. During operation, the objective lens of the microscope 07 extends into the inside of the integrating sphere 16 through the opening for observing the object to be measured placed in the integrating sphere 16. sample. Preferably, the size of the objective lens matches the size of the opening on the integrating sphere 16;

The microscope 07 in the present invention can distinguish individual particles with a size of not less than 100nm in any dimension. Preferably, as an implementable mode, the microscope 07 in the present invention is a stereomicroscope, which has a relatively high resolution and can ensure Realize the luminescence performance test of a single particle. When the sample to be tested contains more than two kinds of particles, the luminescence performance of one of the solid powder particles can be tested first, and then the mobile platform can be adjusted through the observation of the microscope 07, and then the luminescence performance of the other solid powder particle can be tested.

In addition, the present invention also includes a controller 01, which is electrically connected to the excitation light source 05, the mobile platform, the spectrometer 03 and the microscope 07, and is used to control the actions of the excitation light source 05, the mobile platform, the spectrometer 03 and the microscope 07. At the same time, the controller 01 can also receive and analyze the data returned by each component.

As a possible implementation, the mobile platform in the present invention is an omnidirectional mobile platform, which can drive the sample stage 11 to move in all directions. The omnidirectional mobile platform ensures the comprehensiveness of the particle test, especially when the sample to be tested contains many types, the position of the sample to be tested can be moved by the omnidirectional mobile platform to ensure that the performance of each particle can be tested.

Preferably, the omnidirectional mobile platform includes a first electric control platform 15, a second electric control platform 14 and a third electric control platform 13; wherein, the first electric control platform 15 can drive the sample stage 11 to move around the central axis of the sample stage 11 With 360° rotation, the second electric control platform 14 can drive the sample stage 11 to move horizontally along the X-Y direction, and the third electric control platform 13 can drive the sample stage 11 to move vertically along the Z axis direction. Wherein, the first electric control platform 15 , the second electric control platform 14 and the third electric control platform 13 are respectively electrically connected to the controller 01 , and can independently drive the sample stage 11 to perform actions.

The minimum rotation angle of the first electric control platform 15 is less than or equal to 0.5°, and the minimum moving distances of the second electric control platform 14 and the third electric control platform 13 are less than or equal to 1 micron. Higher precision can improve the accuracy of the test.

In order to further increase the accuracy of the test and prevent light leakage and other phenomena during the test, in the present invention, the opening of the integrating sphere 16 is provided with a sealing assembly. When the objective lens of the microscope 07 penetrates into the inside of the integrating sphere 16, the sealing assembly can The gap between the objective lens and the integrating sphere 16 is sealed.

When measuring the thermal quenching properties of the sample to be tested, the temperature of the sample to be tested is usually changed. Therefore, as a possible implementation, the inside of the integrating sphere 16 is also provided with a heating device for heating the sample to be tested on the sample stage 11. A device 12 , the heating device 12 is electrically connected to the controller 01 and operates under the control of the controller 01 . Wherein, the heating device 12 can be a heating plate, and is arranged directly under the sample stage 11, and can continuously heat the sample to be tested from room temperature to 300°C.

Because in the working process, the integrating sphere 16 is in a sealed state, in order to facilitate the observation of the microscope 07, an auxiliary light source 10 is also provided inside the integrating sphere 16. Preferably, the auxiliary light source 10 can be a white LED light source, an incandescent lamp or xenon lamp. In the present invention, the auxiliary light source 10 is electrically connected to the controller 01 and works under the control of the controller 01 . When the excitation light source 05 is in working state, the auxiliary light source 10 is turned off under the control of the controller 01 , and when the position of the sample to be measured is determined by the microscope 07 , the auxiliary light source 10 is turned on under the control of the controller 01 .

The present invention also includes a first guiding optical fiber 02, a second guiding optical fiber 04 and a third guiding optical fiber 08; an optical fiber fixing device 09 is provided inside the integrating sphere 16, and as a possible implementation mode, a fixing tube 06 is also provided inside the integrating sphere 16 , the fiber fixing device 09 is fixedly connected to the integrating sphere 16 through the fixing tube 06, and is arranged above the sample stage 11; one end of the first guiding fiber 02 is connected to the fiber fixing device 09, the other end is connected to the spectrometer 03, and the second guiding fiber 04 One end is connected to the optical fiber fixing device 09, and the other end is connected to the excitation light source 05; the inner wall of the integrating sphere 16 is provided with a light baffle, one end of the third guiding fiber 08 is connected to the light baffle, and the other end is connected to the spectrometer 03.

Preferably, a position sensor is installed on the optical fiber fixing device 09 , and the position sensor is electrically connected to the controller 01 . When using the moving platform to adjust the position of the sample stage 11 , the position sensor effectively avoids the contact between the optical fiber fixing device 09 and the sample stage 11 .

When the present invention is testing, the sample to be tested in the integrating sphere 16 can be observed through the microscope 07, and the sample to be tested can be moved by the mobile platform, so that the solid powder particles at a certain position can be tested specifically, Realize the test of the luminescence performance of a single particle phosphor, for phosphor solid powder particles composed of a variety of different substances, the luminescence properties of each phosphor solid powder particle itself can be directly measured. At the same time, the invention has complete functions, not only can test the photoluminescence property of a single solid powder particle, but also can test the variation of the luminescent property of a single solid powder particle with temperature and the quantum efficiency of a single solid powder particle.

The present invention will be further described below by specific examples.

Example 1

Measurement of photoluminescent properties of phosphor solid powder particles:

1) First open the integrating sphere 16, place the fluorescent powder to be tested in the groove on the sample stage 11, close the integrating sphere 16; turn on the auxiliary light source 10 and the microscope 07 through the controller 01, and adjust the mobile platform through the controller 01, The microscope 07 can clearly observe the sample to be tested on the sample stage 11, and the position sensor installed on the optical fiber fixing device 09 can prevent the mobile platform from rising too much and touching the optical fiber fixing device 09; use the controller 01 to turn on the excitation light source 05 (xenon lamp ), the auxiliary light source 10 is automatically turned off; the controller 01 is used to turn on the spectrometer 03; the controller 01 is used to adjust the mobile platform so that the light emitted by the excitation light source 05 is irradiated on a certain particle of the sample to be tested through the second conductive optical fiber 04, Under the light excitation of the excitation light source 05, the particle emits emitted light, and the emitted light is transmitted to the spectrometer 03 through the first conducting optical fiber 02; the spectrometer 03 transmits the measured signal to the controller 01, and finally the terminal of the controller 01 obtains the Photoluminescence spectra of particles.

2) Constantly use the controller 01 to adjust the position of the mobile platform, so that the light emitted by the excitation light source 05 is irradiated on other particles to be measured through the second conductive optical fiber 04; the irradiated particles emit light under excitation, and pass through the first conductive The optical fiber 02 is conducted to the spectrometer 03; the spectrometer 03 transmits the measured signal to the controller 01, and finally the photoluminescence spectrum of the irradiated particles is obtained at the terminal of the controller 01. As shown in FIG. 2 , it is a photoluminescence spectrum of a phosphor particle measured by the method in this embodiment.

Example 2

Quantum efficiency measurement of phosphor solid powder particles:

1) Firstly mix the phosphor solid powder particles to be measured with a certain amount of barium sulfate powder particles evenly, then open the integrating sphere 16, place the mixed powder particles of phosphor powder and barium sulfate in the groove on the sample stage 11, Close the integrating sphere 16; turn on the auxiliary light source 10 and the microscope 07 through the controller 01, and adjust the mobile platform through the controller 01, so that the microscope 07 can clearly observe the mixed powder particles on the sample stage 11, and the optical fiber fixture 09 installed on the The position sensor can prevent the mobile platform from rising excessively and thus touch the optical fiber fixing device 09; the excitation light source 05 (laser) is turned on by the controller 01, and the auxiliary light source 10 is automatically turned off at this time; the spectrometer 03 is turned on by the controller 01; the movement is adjusted by the controller 01 platform, so that the light emitted by the excitation light source 05 is irradiated on a certain barium sulfate particle in the mixed powder particles through the second conductive optical fiber 04, and the barium sulfate particle reflects the light emitted by the excitation light source 05, and the reflected light passes through the third conductive optical fiber 08 Conducted to the spectrometer 03; the spectrometer 03 transmits the measured signal to the controller 01 to obtain a reference spectrum.

2) Use the controller 01 to adjust the mobile platform so that the light emitted by the excitation light source 05 is irradiated on a certain phosphor particle in the mixed powder particles through the second conductive optical fiber 04, and the phosphor particle emits emission under the excitation of the excitation light source 05 The emitted light is transmitted to the spectrometer 03 through the third conducting optical fiber 08; the spectrometer 03 transmits the measured signal to the controller 01, and finally obtains the photoluminescence spectrum of the phosphor particle.

3) By calculating the reference spectrum obtained in step 1) and the photoluminescence spectrum obtained in step 2), the quantum efficiency of a phosphor particle tested in step 2) is finally obtained.

4) Constantly use the controller 01 to adjust the position of the mobile platform, so that the light emitted by the excitation light source 05 is irradiated on other phosphor particles in the mixed powder particles through the second conductive optical fiber 04, and the irradiated particles emit light under excitation, Conducted to the spectrometer 03 through the third conducting optical fiber 08; the spectrometer 03 transmits the measured signal to the controller 01, through the reference spectrum obtained in step 1), and finally obtains the quanta of the irradiated particles at the terminal of the controller 01 efficiency. As shown in FIG. 3 , it is a quantum efficiency spectrum of a phosphor particle measured by the method in this embodiment.

Example 3

Measurement of Thermal Quenching Properties of Phosphor Solid Powder Particles:

1) First open the integrating sphere 16, place the fluorescent powder to be tested in the groove on the sample stage 11, close the integrating sphere 16; turn on the auxiliary light source 10 and the microscope 07 through the controller 01, and adjust the mobile platform through the controller 01, The microscope 07 can clearly observe the sample to be tested on the sample stage 11, and the position sensor installed on the optical fiber fixing device 09 can prevent the mobile platform from rising too much and touching the optical fiber fixing device 09; use the controller 01 to turn on the excitation light source 05 (LED light), at this time the auxiliary light source 10 is automatically turned off; use the controller 01 to turn on the spectrometer 03; use the controller 01 to control the heating device 12 to work, so that the temperature of the heating device 12 rises to the preset temperature value and keeps it for 10 minutes, so that the sample stage 11 The temperature of the sample to be tested in the groove is consistent with the preset temperature value of the heating device 12; use the controller 01 to adjust the mobile platform so that the light emitted by the excitation light source 05 is irradiated to a certain particle of the sample to be tested through the second conductive optical fiber 04 Above, the particle emits emitted light under the light excitation of the excitation light source 05, and the emitted light is transmitted to the spectrometer 03 through the first guide optical fiber 02; the spectrometer 03 transmits the measured signal to the controller 01, and finally at the terminal of the controller 01 A photoluminescence spectrum of the particle was obtained.

2) Continue to use the controller 01 to control the heating device 12 for heating, so that the temperature of the heating device 12 is changed to another preset temperature value and kept for 10 minutes, so that the temperature of the sample to be tested in the groove on the sample stage 11 is the same as that of the heating device 12 The other preset temperature value is consistent; the light emitted by the excitation light source 05 is irradiated on the phosphor particles measured in step 1) through the second conductive optical fiber 04, and the particles emit emitted light under the light excitation of the laser light source, and the emitted light passes through The first guide fiber 02 is conducted to the spectrometer 03; the spectrometer 03 transmits the measured signal to the controller 01, and finally the photoluminescence spectrum of the phosphor particles at the temperature is obtained at the terminal of the controller 01.

3) Repeat step 2), change the preset temperature value, count the collected spectral data, and finally obtain the thermal quenching map of a certain particle of the phosphor. As shown in FIG. 4 , it is a thermal quenching spectrum of a phosphor particle measured by the method in this embodiment.

It should be noted that the device of the present invention can not only measure the luminescence performance of a single solid powder particle, but also can measure the luminescence performance of a macroscopic solid powder particle. The specific test method is the same as the traditional test method, and will not be repeated here. .

The above embodiments only provide several implementation modes of the present invention, and other variations and improvements can also be provided.

Claims (10)

1. The luminescent material performance testing device based on the mobile platform is characterized in that it comprises an excitation light source, a spectrometer, an integrating sphere, a microscope and a controller; the inside of the integrating sphere is provided with a sample stage and a mobile platform, and the sample stage is used to place the Measure the sample, and the mobile platform is used to drive the sample stage to move; The integrating sphere is provided with an opening, and during operation, the objective lens of the microscope extends into the integrating sphere through the opening for observing the sample to be measured placed in the integrating sphere; The controller is electrically connected with the excitation light source, the mobile platform, the spectrometer and the microscope respectively, and is used to control the actions of the excitation light source, the mobile platform, the spectrometer and the microscope. 2 . The mobile platform-based luminescent material performance testing device according to claim 1 , wherein the microscope is a stereomicroscope capable of distinguishing particles with a size not smaller than 100 nm in any dimension. 3. The device for testing the performance of luminescent materials based on a mobile platform according to claim 1, wherein the mobile platform is an omnidirectional mobile platform, and the omnidirectional mobile platform can drive the sample stage to move in all directions. 4. The mobile platform-based luminescent material performance testing device according to claim 1, wherein the omnidirectional mobile platform comprises a first electric control platform, a second electric control platform and a third electric control platform; The first electric control platform drives the sample stage to rotate 360° around its central axis, the second electric control platform drives the sample stage to move horizontally along the X-Y direction, and the third electric control platform drives the sample stage along the Z axis direction to move vertically. 5. The mobile platform-based luminescent material performance testing device according to claim 4, characterized in that the minimum rotation angle of the first electric control platform is less than or equal to 0.5°, and the second electric control platform and the third electric control platform The minimum moving distance is less than or equal to 1 μm. 6. The device for testing the performance of luminescent materials based on a mobile platform according to claim 1, wherein a sealing assembly is provided at the opening, and when the objective lens of the microscope extends into the inside of the integrating sphere, the sealing assembly will The gap between the objective lens and the integrating sphere is sealed. 7. The mobile platform-based luminescent material performance testing device according to claim 1, wherein a heating device is provided inside the integrating sphere, the heating device is electrically connected to the controller, and the heating device is used to heat the sample stage samples to be tested. 8. The mobile platform-based luminescent material performance testing device according to claim 1, wherein an auxiliary light source is provided inside the integrating sphere, and the auxiliary light source is electrically connected to the controller. 9. The luminescent material performance testing device based on the mobile platform according to claim 1, further comprising a first guiding fiber, a second guiding fiber and a third guiding fiber; An optical fiber fixing device is also provided inside the integrating sphere; one end of the first guiding fiber is connected to the fiber fixing device, the other end of the first guiding fiber is connected to the spectrometer, one end of the second guiding fiber is connected to the fiber fixing device, and the second The other end of the conducting fiber is connected to the excitation light source; A light baffle is provided on the inner wall of the integrating sphere, one end of the third guiding fiber is connected to the light baffle, and the other end of the third guiding fiber is connected to a spectrometer. 10 . The mobile platform-based luminescent material performance testing device according to claim 9 , wherein a position sensor is provided on the optical fiber fixing device, and the position sensor is electrically connected to the controller. 11 .