Disclosure of Invention
The invention provides an array sample spectrum testing system, which comprises:
a sample stage for carrying an array sample;
the light source unit is arranged above the sample table to optically excite the sample, the light source unit is provided with a plurality of light sources which are arranged in parallel or in an array, and the distance between the plurality of light sources is matched with the distance between the array samples;
the detector units are arranged above the sample table, the spacing between the detector units is matched with the spacing between the array samples, and when the detector units are aligned with the corresponding samples, the spectral data of the samples are obtained through testing; and
and the master control computer is connected with the plurality of detector units and records and displays the spectrum data.
Further, each of the detector units includes:
the coupling lens is arranged above the sample table and faces the sample; and
the optical fiber spectrometer is connected with the coupling lens through an optical fiber and is electrically connected with the master control computer, so that spectral data obtained by processing the optical signal obtained by the coupling lens is transmitted to the master control computer.
Further, the detector unit comprises an optical filter arranged between the sample stage and the coupling lens.
Further, the coupling lens is vertically arranged, the angle between the light source unit and the horizontal plane is 30-60 degrees, and the coupling lens and the lower end of the light source unit are located at the same height.
Furthermore, a spectrum calibration device is arranged between the coupling lens and the optical fiber spectrometer, and the spectrum calibration device comprises a slit with adjustable width and optical fiber collimating mirrors arranged at two ends of the slit.
Further, the light source unit includes a slot and a modularized light source group or a light source array, and the light source group or the light source array is inserted into the slot.
Furthermore, the slot is obliquely arranged, a magnet is arranged in the slot, and the magnet is also arranged at the position of the light source group or the light source array corresponding to the slot, so that when the light source group or the light source array is inserted into the slot, the corresponding magnets attract each other to fix the light source group or the light source array in the slot.
Furthermore, the array sample spectrum testing system further comprises a sample stage moving unit arranged at the lower part of the sample stage, and the sample stage moving unit is connected with the main control computer so as to control the sample stage moving unit to move through the main control computer.
Furthermore, the array sample spectrum testing system also comprises a mobile station controller connected between the main control computer and the sample stage moving unit, and the mobile station controller receives the instruction sent by the main control computer and controls the sample stage moving unit to move.
The invention has the following effects:
on one hand, the invention adopts the optical fiber spectrometer, so that the speed of obtaining the spectral curve is dozens of times faster than that of a conventional fluorescence photometer; moreover, the light source of the array and the corresponding spectrometer unit can multiply the efficiency of the spectrum test; in addition, data tested by multiple channels simultaneously can be displayed and compared intuitively through software at the same time, so that the intuitiveness and the efficiency of test screening are improved;
on the other hand, the invention also solves the problems when the combination is applied to the rapid spectrum test: firstly, the invention adopts a modularized light source and a slot-in type light source fixing device, which not only solves the problem that excitation sources need to be replaced midway when excitation wavelengths of different fluorescent samples are different, but also ensures that the positions of the light source and the coupling lens are relatively fixed, thereby increasing the stability of the test; secondly, when a fluorescent material sample for spectrum test is placed on a sample table, the difference in spectrum intensity is often caused by the difference in amount or position, and each optical fiber spectrometer in the invention is provided with an independent spectrum calibration device to adjust the luminous flux, so that the adjustment can be conveniently carried out according to the requirement, and the accuracy and the consistency of the measurement can be ensured.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting thereof.
FIG. 1 shows the structure of an array sample spectrum test system in this embodiment. As shown in fig. 1 and 2, the array sample spectrum test system of the present invention includes: a sample stage 106 on which an array sample is placed; a light source unit 101 disposed above the sample stage 106 to optically excite the sample, the light source unit 101 having a plurality of light sources arranged in parallel or in an array, and a pitch between the plurality of light sources matching a pitch between the array samples; a plurality of detector units disposed above the sample stage 106, the plurality of detector units corresponding to the plurality of light sources for detecting a spectrum of the sample; a sample stage moving unit 107 provided at a lower portion of the sample stage 106, for moving a position of the sample stage 106; a stage controller 108 connected to the stage moving unit 107, for controlling the stage moving unit 107 to move the sample stage 106; and a main control computer 109 connected to and controlling the mobile station controller 108 and the plurality of detector units.
Each detector unit comprises: a coupling lens 102 disposed above the sample stage 106 and facing the sample for receiving the optical signal; an optical filter 105 disposed between the sample and the coupling lens 102 for removing interference signals; and a fiber spectrometer 104 connected to the coupling lens 102 through an optical fiber 103, for processing the optical signal to obtain spectral data, including collimating, dispersing, focusing, projecting, photoelectric converting, counting, etc. the optical signal. The fiber spectrometer 104 of the detector unit transmits the processed spectral information to the main control computer 109, and the processed spectral information is converted into an image by the main control computer 109 and is recorded and displayed. Processing and converting the optical signal into an image is prior art, and therefore will not be described herein. After the plurality of detector units complete the test on the corresponding plurality of samples, the main control computer 109 sends a moving instruction with a next test position to the mobile station controller 108, so that the mobile station controller 108 controls the sample stage moving unit 107 to move the sample stage 106 to the specified next test position, that is, the plurality of detector units are aligned with the positions of the plurality of samples to be tested, and then the test is started through the detector units again, thereby realizing the automatic traversal spectrum test on each sample on the sample stage under the control of the main control computer.
In this embodiment, the array sample may be an independent sample including { a × B } ordered arrays, and may be a powder, film material, or bulk sample. The sample to be tested is prepared or assembled on the base plate in an array form, the base plate is detachably arranged on the sample table, the base plate is placed on the sample table and fixed during testing, and the base plate can be independently detached to prepare or assemble the sample when the sample is not tested. The spacing distance of each sample in the array sample on the substrate is matched with the spacing distance of the plurality of detector units, so that the plurality of light sources can excite and test the plurality of samples simultaneously, and the spectrum testing efficiency is greatly improved.
The sample stage moving unit 107 carries the sample stage 106 and moves the array samples to match the positions of the spectroscopic test sites. Preferably, the sample stage moving unit 107 includes a transverse motor driving device and a longitudinal motor driving device connected to the sample stage 106, the two motor driving devices respectively move the sample stage 106 in the horizontal transverse direction and the horizontal longitudinal direction, and the motor driving device is a servo motor or a stepping motor. The moving distance of the sample stage 106 can be set according to requirements. The mobile station controller 108 is used for receiving the command from the main control computer 109 and controlling the direction and the number of steps of the motor operation. Specifically, the mobile station controller 108 is a stepping motor controller, and since the main control computer generally cannot directly control the stepping motor, the mobile station controller 108 can be configured to perform command conversion.
Referring to fig. 2 to 4, fig. 3 is a schematic diagram of a side view and a rear view of fig. 2, and fig. 4 is a schematic diagram of the light source inserted into the slot along a direction indicated by an arrow in fig. 2. The light source of the light source unit 101 is a plurality of laser light sources or LED light sources arranged in parallel or in an array. Preferably, the light source is a modular set or array of light sources. The light source unit 101 has a fixed casing, the casing is cube-shaped, an opening is formed on one side of the casing far away from the coupling lens, and a slot for fixing the light source is formed in the casing, so as to facilitate the replacement and positioning of the light source, the size of the modularized light source group or light source array is matched with the size of the slot, the light source group or light source array is inserted into the slot when in use, and a uniform plug-in power supply is provided, thereby facilitating the replacement of the light source with different wavelengths, and facilitating the positioning of the light source relative to the light source unit 101 while the light source unit 101 is suitable for optical excitation of different sample materials. The light source can be a laser light source with wavelengths from near ultraviolet to near infrared such as 365nm, 404nm, 450nm, 545nm, 665nm, 808nm and 980nm, and other types of light sources can be customized according to needs.
Further, the slot is disposed obliquely, and the angle between the light source and the horizontal plane after the light source is inserted into the slot is 30 ° to 60 °, and preferably about 45 °. The inclined slot is internally provided with an inclined plane, four corners of the inclined plane are provided with magnets, and the positions of the light source corresponding to the four corners are also provided with magnets, so that when the light source is inserted into the slot, the magnets in the slot and the magnets on the light source attract each other to play a role in positioning and fixing the light source, and meanwhile, the light source can be conveniently taken out or inserted into the slot for fixing. More specifically, the light source is fixed to the lower surface of the inclined plane. Different light source groups or light source arrays are provided with uniform power interfaces, and when the LED light source module needs to be used, the light source groups or the light source arrays are inserted into the slots and then are connected with a power supply through the power interfaces.
The coupling lens 102 is fixed vertically, and the coupling lens 102 is located at substantially the same height as the lower end of the light source unit 101 and at a distance of about 1-2cm from the upper surface of the sample stage 106.
The optical filter 105 can filter out interference signals generated by the excitation light source or other factors, improve the signal-to-noise ratio of the spectrometer, and can select a long-wave-pass or short-wave-pass optical filter according to requirements. The filter 105 is positioned below the coupling lens 102 by a magnet.
The fiber spectrometer 104 is connected to the coupling lens 102 through the optical fiber 103, so that the position of the fiber spectrometer 104 can be flexibly set, and considerable convenience is brought to the design of a test system. Preferably, the number of pixels of the fiber spectrometer 104 is 2048 and above. The number of pixels is the number of CCD array detectors in the fiber spectrometer, the number of pixels is the data amount of the spectrum data obtained by testing, and the more the number of pixels is, the higher the resolution of the spectrum testing is. The resolution of the spectrum test can reach 1.0nm and above by selecting the fiber spectrometer with the pixel number of 2048 and above. The fiber spectrometer 104 is also provided with an ultraviolet enhancement window, the CCD detector without the ultraviolet enhancement window has a very low response to optical signals with a wavelength less than 350nm, and the ultraviolet enhancement window can enhance the signal response of the system to this band. Therefore, the measurement range of the spectrum test system can reach 200-1100 nm. The slit width of the fiber optic spectrometer 104 is less than 50 microns. The slit width determines the width of the beam incident into the spectrometer and is an important factor affecting the optical resolution of the spectrometer. By selecting an entrance slit having a width of 50 μm or less, an optimum optical resolution of 0.4nm or more can be obtained.
It should be noted that, when the same sample to be tested is tested in different test channels, the intensities of the sample may differ, and in order to ensure the test consistency of different channels, the optical signal received by the coupling lens needs to be calibrated, and the signal intensities of different channels are changed to make the signal intensities consistent. Therefore, as a preferred embodiment of the present invention, a spectrum calibration device 110 is disposed between the coupling lens 102 and the fiber spectrometer 104, and the spectrum calibration device 110 includes a slit with adjustable width and fiber collimating mirrors disposed at two ends of the slit. The slit is similar to the structure of a baffle plate and is used for shielding a part of optical signals to change the light intensity, and the slit is continuously adjustable by 0-100%. The function of the fiber collimating mirror is to keep the same direction of the light entering and exiting, and reduce unnecessary optical signal loss. The wavelength range of the optical signal that this spectrum calibration device can handle is 200~2500 nm.
The main control computer comprises a testing module, an operating module, a storage module and a display module which are connected with each other, the testing module is connected with the optical fiber spectrometer 104 and used for a user to input sample testing parameters, the optical fiber spectrometer 104 processes obtained optical signals of samples according to the input sample testing parameters to obtain spectrum data, the storage module is used for storing the spectrum data, and the display module is used for displaying the spectrum data. The operation module is connected with the mobile station controller 108 and is used for inputting an operation instruction by a user, when the operation module automatically sends a moving instruction with a next test position to the mobile station controller 108 after the storage module stores spectral data, so that the mobile station controller 108 calculates the running direction and the running steps of the motor according to the next test position, and the sample stage moving unit 107 moves the sample stage 106; when manually operated, the user inputs the next test position to the manipulator module, which in turn sends a move command with the next test position to the mobile station controller 108.
The following describes the procedure for testing using the array sample spectroscopic test system described above:
firstly, a sample to be tested is loaded into a sample table 106 in an array form, a light source which is needed to be used as exciting light in a light source unit 101 is replaced according to the tested sample, a needed optical filter 105 is replaced, sample testing parameters (spectral range, exciting illumination time and the like) of a corresponding position are set in a main control computer 109, after the test is started, the light source of the light source unit 101 emits exciting light to irradiate the sample, the sample is excited to emit a spectral signal, the spectral signal is filtered by the optical filter 105, received by a coupling lens 102 and then transmitted into an optical fiber spectrometer 104 through an optical fiber 103, the spectral signal is subjected to collimation, dispersion, focusing, photoelectric conversion and other treatments by the optical fiber spectrometer 104, the treated spectral information is transmitted to the main control computer 109, and the processed spectral information is converted into an image by the main control computer 109 and is recorded and displayed; after the testing of one group of samples is completed, the main control computer 109 sends a moving command with a next testing position to the mobile station controller 108, and the mobile station controller 108 controls the sample station moving unit 107 to move to a specified next testing position, at which time the detector unit starts the testing of the next group of samples.
The invention can simultaneously carry out spectrum test on a plurality of samples according to the requirement, realizes multichannel parallel spectrum test, can be used for rapid spectrum test of array samples in material genetic engineering, can obtain the spectrum data of a large number of samples at one time, and greatly improves the research and development efficiency of materials. The invention has extremely high signal processing speed, can simultaneously and quickly finish the emission spectrum test, the record and the spectrum superposition comparison of a plurality of samples, displays the wavelength peak value numerical value of the emission spectrum of the sample, the color coordinate graph and the coordinate value of the emission spectrum, and then screens out the optimal sample by a large amount of reusable spectrum data. The excitation light source can be conveniently replaced, the optical fiber spectrometer is adopted, the movement of the sample table is controlled by the main control computer, the controllable adjustment of parameters such as the excitation wavelength, the measurement range, the sample position and the like is realized, and the technical requirements of efficient screening and optimization of test parameters are met.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
The spectral test experiment was performed on a single phosphor sample according to the array sample spectral test system shown in fig. 1. According to the requirements, an excitation light source and a corresponding optical fiber spectrometer combination are adopted, the number of pixels of the optical fiber spectrometer is 2048, the spectral measurement range is 300-1000nm, the slit width is 50 microns, the excitation wavelength is 370nm near ultraviolet LED light source, and the optical filter is a 440nm long-wave pass optical filter.
FIG. 5 shows experimental results of a single phosphor sample tested using the array sample spectroscopic test system designed and manufactured in FIG. 1. As can be seen, under the irradiation of 370nm LED light source, the phosphor emits yellow fluorescence with a central wavelength of about 580 nm. Fig. 6 shows a color coordinate diagram of the emission spectrum, and it can be seen that the spectral region of the emission spectrum is located in the yellow and orange regions, and the color coordinate values are about (0.53, 0.40).
EXAMPLE 2
A set of three identical phosphor samples were subjected to a spectroscopic testing experiment with an array sample spectroscopic testing system designed and manufactured according to fig. 1. According to the requirements, one, two or three excitation light sources and corresponding fiber spectrometer combinations are adopted, the number of pixels of the fiber spectrometer is 2048, the spectral measurement range is 300-1000nm, the slit width is 50 microns, the excitation wavelength is 980nm near-infrared laser light source, and the optical filter is 785nm short-wave pass optical filter.
FIG. 7 shows the experimental results of a set of three identical phosphor samples tested using the array sample spectral testing system designed and manufactured in FIG. 1. As can be seen from the graph, the spectrum range of the obtained experimental result is 300-1000nm, and the spectrum intensity values and curve shapes of the three light beams have consistency, which indicates that the array sample spectrum testing system of the invention has stability in measurement. Thus, it is convenient to visually compare and screen multiple samples as compared to, for example, example 1, performing an experiment on a single sample.
Example 3
A set of three fluorescent ceramic wafer samples of the same type but different luminous efficiencies were subjected to a spectrum test experiment with an array sample spectrum test system designed and manufactured according to fig. 1. According to the requirements, three excitation light sources and corresponding fiber spectrometer combinations are adopted, the number of pixels of the fiber spectrometer is 2048, the spectral measurement range is 300-1000nm, the slit width is 50 microns, the excitation wavelength is 450nm LED light source, and the optical filter is a 480nm long-wave pass optical filter.
Fig. 8 shows the experimental results of a set of three samples of the same type of fluorescent ceramic chip with different luminous efficiencies tested by the spectral testing system designed and manufactured by the array sample of fig. 1. As can be seen from the graph, the spectral range of the obtained experimental result is 300-1000nm, the spectral intensity values of the three light beams are different, but the curve shapes are consistent. Thus, it is convenient to visually compare and screen multiple samples as compared to, for example, example 1, performing an experiment on a single sample.
Example 4
The spectral test experiment was performed on a {6 × 9} sample of arrayed fluorescent materials with an arrayed sample spectral test system designed and manufactured according to fig. 1. Three excitation light sources and corresponding fiber spectrometer combinations are adopted, the number of pixels of the fiber spectrometer is 2048, the spectral measurement range is 300-1000nm, and the slit width is 50 microns. During the test process, the corresponding excitation light source and the corresponding optical filter are replaced according to different samples.
FIG. 9 shows an interface of a host computer where a user can operate to issue move commands, in this embodiment, 54 samples of a {6 × 9} array are divided into 18 groups, and in the case of automatic testing, the system performs traversal tests on the samples in the order of (1,2,3), (4,5,6) … (52,53, 54); in the case of manual operation, the corresponding position button can be manually clicked, the system will automatically move to the corresponding position, and then test is performed as needed. For example, as shown in fig. 10, when the position is displayed as "456" in performing an automatic test, or "456" in the interface shown in fig. 9 is manually selected, the mobile station controller controls the mobile station to move so that the three detector units are aligned with samples numbered 4,5, and 6, respectively, and perform a test. Fig. 11 shows the experimental results of the test at the position of fig. 10.
As the present invention may be embodied in several forms without departing from the spirit of essential characteristics thereof, the present embodiments are therefore illustrative and not restrictive, since the scope of the invention is defined by the appended claims rather than by the description herein, and all changes that fall within metes and bounds of the claims, or equivalence of such metes and bounds thereof are therefore intended to be embraced by the appended claims.