CN106644858B - A kind of laser particle size analyzer and particle size distribution testing method - Google Patents
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Abstract
Description
技术领域technical field
本发明涉及仪器仪表技术领域,特别涉及一种激光粒度仪,还涉及一种粒度分布测试方法。The invention relates to the technical field of instruments and meters, in particular to a laser particle size analyzer, and also to a particle size distribution testing method.
背景技术Background technique
激光粒度仪是根据颗粒能使激光产生衍射或散射得到散射谱测试粒度分布以及颗粒大小的仪器。其具体工作原理如下:由于激光具有很好的单色性和极强的方向性,所以一束平行的激光在没有阻碍的无限空间中将会照射到无限远的地方,并且在传播过程中很少有发散的现象;当光束遇到颗粒阻挡时,一部分光将发生散射现象,散射光的传播方向将与主光束的传播方向形成一个夹角θ。散射理论和实验结果都告诉我们,散射角θ的大小与颗粒的大小有关,颗粒越大,产生的散射光的θ角就越小;颗粒越小,产生的散射光的θ角就越大。与此同时,散射光的强度代表该粒径颗粒的数量。在不同的角度上测量散射光的强度,就可以得到样品的粒度分布了。The laser particle size analyzer is an instrument for testing the particle size distribution and particle size based on the particle's ability to diffract or scatter laser light to obtain a scattering spectrum. Its specific working principle is as follows: Since the laser has good monochromaticity and strong directionality, a beam of parallel laser light will irradiate to an infinite distance in an infinite space without hindrance, and it will be very fast during the propagation process. There is little divergence; when the beam is blocked by particles, part of the light will be scattered, and the propagation direction of the scattered light will form an angle θ with the propagation direction of the main beam. Scattering theory and experimental results tell us that the size of the scattering angle θ is related to the size of the particle. The larger the particle, the smaller the θ angle of the scattered light; the smaller the particle, the larger the θ angle of the scattered light. At the same time, the intensity of scattered light represents the number of particles of that size. By measuring the intensity of scattered light at different angles, the particle size distribution of the sample can be obtained.
现有的技术中,市场上销售的大部分的激光粒度仪产品利用硅光电二极管或者CCD、CMOS等光电原件作为探测器。硅光电二极管探测器可以直接对圆环探测单元接收到的光电信号进行后期的信号处理,缺点是直接利用CCD或CMOS等光电原件,需要在系统中添加对中调整程序,占用计算机运算内存,降低运算速度,操作复杂。In the existing technology, most of the laser particle size analyzers sold on the market use photoelectric elements such as silicon photodiodes or CCDs and CMOSs as detectors. The silicon photodiode detector can directly process the photoelectric signal received by the ring detection unit in the later stage. The disadvantage is that it directly uses photoelectric components such as CCD or CMOS, and needs to add a centering adjustment program to the system, occupying computer computing memory, and reducing Computing speed, complex operation.
因此,如何提高粒度分布运算速度是本领域技术人员需要解决的技术问题。Therefore, how to improve the calculation speed of the particle size distribution is a technical problem to be solved by those skilled in the art.
发明内容Contents of the invention
本发明的目的是提供一种激光粒度仪,利用圆环掩膜板获取电荷耦合光电探测器接收散射光的像素点对应的位置,进而提高粒度分布运算速度。The object of the present invention is to provide a laser particle size analyzer, which uses a ring mask to obtain the corresponding position of the pixel point where the charge-coupled photodetector receives scattered light, thereby increasing the calculation speed of the particle size distribution.
为解决上述技术问题,本发明提供一种激光粒度仪,包括:In order to solve the above technical problems, the present invention provides a laser particle size analyzer, comprising:
用于发射激光光束的激光光源;a laser light source for emitting a laser beam;
用于盛放待测样品的样品池;A sample cell for holding the sample to be tested;
用于接收所述激光光束穿过所述待测样品后产生的散射光,并将其转换为散射光能量分布图,表面设置有圆环掩膜板的电荷耦合光电探测器;A charge-coupled photodetector for receiving the scattered light generated after the laser beam passes through the sample to be tested, and converting it into a scattered light energy distribution diagram, with a ring mask on the surface;
用于根据所述散射光能量分布图计算所述待测样品的粒度分布的计算器。A calculator for calculating the particle size distribution of the sample to be tested according to the scattered light energy distribution diagram.
优选的,在上述激光粒度仪中,所述圆环掩膜板包括多个同心圆环,最小半径圆环的中心与所述电荷耦合光电探测器的光学中心重合。Preferably, in the above-mentioned laser particle size analyzer, the ring mask includes a plurality of concentric rings, and the center of the ring with the smallest radius coincides with the optical center of the charge-coupled photodetector.
优选的,在上述激光粒度仪中,还包括设置于所述激光光源与所述样品池之间的准直扩束装置。Preferably, the above-mentioned laser particle size analyzer further includes a collimating beam expander arranged between the laser light source and the sample cell.
优选的,在上述激光粒度仪中,所述准直扩束装置为开普勒式激光扩束装置,包括会聚透镜和准直透镜。Preferably, in the above-mentioned laser particle size analyzer, the collimating beam expanding device is a Keplerian laser beam expanding device, including a converging lens and a collimating lens.
优选的,在上述激光粒度仪中,还包括位于所述会聚透镜的焦点处的空间滤波器。Preferably, in the above-mentioned laser particle size analyzer, a spatial filter located at the focal point of the converging lens is further included.
优选的,在上述激光粒度仪中,还包括设置于所述样品池与所述光电探测器之间的成像透镜,所述成像透镜的焦点与所述光电探测器的中心重合。Preferably, the above-mentioned laser particle size analyzer further includes an imaging lens arranged between the sample cell and the photodetector, the focal point of the imaging lens coincides with the center of the photodetector.
本发明还包括一种粒度分布测试方法,包括:The present invention also includes a particle size distribution testing method, comprising:
步骤S1:将圆环掩膜板设置于激光粒度仪的电荷耦合光电探测器上,调整最小半径圆环的中心与所述电荷耦合光电探测器的光学中心重合;Step S1: setting the ring mask on the charge-coupled photodetector of the laser particle size analyzer, and adjusting the center of the ring with the smallest radius to coincide with the optical center of the charge-coupled photodetector;
步骤S2:激光光源发射的激光光束通过放有待测样品的样品池,形成散射光;Step S2: The laser beam emitted by the laser light source passes through the sample cell containing the sample to be tested to form scattered light;
步骤S3:所述电荷耦合光电探测器接收所述散射光,根据所述圆环掩膜板获取接收所述散射光的像素点的坐标;Step S3: the charge-coupled photodetector receives the scattered light, and obtains the coordinates of the pixel point receiving the scattered light according to the circular mask;
步骤S4:根据所述像素点的坐标绘出所述散射光能量分布图,并计算所述待测样品的粒度分布。Step S4: draw the scattered light energy distribution diagram according to the coordinates of the pixel points, and calculate the particle size distribution of the sample to be tested.
优选的,在上述粒度分布测试方法中,所述步骤S2之前,还包括:Preferably, in the above particle size distribution testing method, before the step S2, it also includes:
步骤S11:调整所述圆环掩膜板中最小半径圆环的中心与所述电荷耦合光电探测器的光学中心重合;Step S11: adjusting the center of the circle with the smallest radius in the circle mask to coincide with the optical center of the charge-coupled photodetector;
步骤S12:所述激光光束通过没有所述放置待测样品的所述样品池,入射至所述电荷耦合光电探测器上;Step S12: the laser beam is incident on the charge-coupled photodetector through the sample cell without the sample to be tested;
步骤S13:判断所述激光光束在所述电荷耦合光电探测器上的光斑是否落在所述最小半径圆环的中心,若否,则调整所述激光光束在所述电荷耦合光电探测器上的对中,若是,则执行所述步骤S2。Step S13: judging whether the spot of the laser beam on the charge-coupled photodetector falls on the center of the circle with the smallest radius, if not, adjusting the spot of the laser beam on the charge-coupled photodetector If yes, execute the step S2.
本发明提供了一种激光粒度仪,包括:用于发射激光光束的激光光源;用于盛放待测样品的样品池;用于接收所述激光光束穿过所述待测样品后产生的散射光,并将其转换为散射光能量分布图的,表面设置有圆环掩膜板的电荷耦合光电探测器;用于根据所述散射光能量分布图计算所述待测样品的粒度分布的计算器。本发明使用圆环掩膜板的目的是更加直观的获取接收散射光的各个像素点对应的位置,便于根据各个像素点对应的位置对散射光能量能量的提取,进而快速绘制散射光能量分布图,加快计算所述待测样品的粒度分布的运算速度。The invention provides a laser particle size analyzer, comprising: a laser light source for emitting a laser beam; a sample cell for holding a sample to be tested; and a sample pool for receiving the scattered light generated after the laser beam passes through the sample to be tested. Light, and convert it into a scattered light energy distribution map, a charge-coupled photodetector with a ring mask plate on the surface; used to calculate the particle size distribution of the sample to be measured according to the scattered light energy distribution map device. The purpose of using the ring mask in the present invention is to obtain the position corresponding to each pixel point receiving scattered light more intuitively, to facilitate the extraction of scattered light energy energy according to the position corresponding to each pixel point, and then to quickly draw the scattered light energy distribution diagram to speed up the calculation speed of calculating the particle size distribution of the sample to be tested.
本发明还提供了一种粒度分布测试方法,具有上述效果。The invention also provides a particle size distribution testing method, which has the above effects.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据提供的附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only It is an embodiment of the present invention, and those skilled in the art can also obtain other drawings according to the provided drawings without creative work.
图1为本发明实施例所提供的激光粒度仪示意图;Fig. 1 is the schematic diagram of the laser particle size analyzer provided by the embodiment of the present invention;
图2为本发明实施例所提供的表面设置有圆环掩膜板的电荷耦合光电探测器示意图;FIG. 2 is a schematic diagram of a charge-coupled photodetector provided with a ring mask on the surface provided by an embodiment of the present invention;
图3为本发明实施例所提供的粒度分布测试方法示意图。Fig. 3 is a schematic diagram of a particle size distribution testing method provided by an embodiment of the present invention.
具体实施方式Detailed ways
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments It is a part of embodiments of the present invention, but not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
请参考图1和图2,图1为本发明实施例所提供的激光粒度仪示意图;图2为本发明实施例所提供的表面设置有圆环掩膜板的电荷耦合光电探测器示意图。Please refer to Figure 1 and Figure 2, Figure 1 is a schematic diagram of a laser particle size analyzer provided by an embodiment of the present invention; Figure 2 is a schematic diagram of a charge-coupled photodetector provided with a ring mask on the surface provided by an embodiment of the present invention.
在一种具体的实施方式中,本发明提供一种激光粒度仪,包括:In a specific embodiment, the present invention provides a laser particle size analyzer, comprising:
用于发射激光光束的激光光源1;A laser light source 1 for emitting a laser beam;
用于盛放待测样品的样品池3;A sample cell 3 for holding the sample to be tested;
用于接收所述激光光束穿过所述待测样品后产生的散射光,并将其转换为散射光能量分布图,表面设置有圆环掩膜板的电荷耦合光电探测器5;Used to receive the scattered light generated after the laser beam passes through the sample to be tested, and convert it into a scattered light energy distribution map, and a charge-coupled photodetector 5 with a ring mask on the surface;
用于根据所述散射光能量分布图计算所述待测样品的粒度分布的计算器6。A calculator 6 for calculating the particle size distribution of the sample to be tested according to the scattered light energy distribution diagram.
具体的,本实施例提供的激光粒度仪,其具体设置方式以及工作方式请参考现有技术,在此不再赘述。用电荷耦合光电探测器5替代硅光电二极管组成的探测器,可以实现被测粒径范围内全数据的采集,不再受光刻技术、加工工艺等的局限,具有更加广泛地应用。Specifically, for the laser particle size analyzer provided in this embodiment, please refer to the prior art for its specific setting method and working method, and details will not be repeated here. Using the charge-coupled photodetector 5 to replace the detector composed of silicon photodiodes can realize the collection of all data within the range of the measured particle size, which is no longer limited by photolithography technology and processing technology, and has a wider range of applications.
电荷耦合光电探测器5是利用内光电效应取得光电转换产生信号电荷的光电器件,其是由多个电荷耦合单元组成的。以金属氧化物半导体晶体管(英文名称:Metal OxideSemiconductor,简称MOS)电容器作为其基本单元。MOS电容器是用氧化的方法在P型或N型硅衬底的表面上生成一层二氧化硅层,然后在二氧化硅层上蒸镀一层金属膜,最后以光刻的方法制成栅状电极,这样就构成MOS电容转移器件,其单个MOS电容器就是CCD探测器的一个像素或一个光敏元。The charge-coupled photodetector 5 is an optoelectronic device that utilizes the internal photoelectric effect to achieve photoelectric conversion to generate signal charges, and is composed of multiple charge-coupled units. A metal oxide semiconductor transistor (English name: Metal Oxide Semiconductor, MOS for short) capacitor is used as its basic unit. MOS capacitors are oxidized to form a silicon dioxide layer on the surface of a P-type or N-type silicon substrate, and then a metal film is evaporated on the silicon dioxide layer, and finally the gate is made by photolithography. Shaped electrodes constitute a MOS capacitive transfer device, and its single MOS capacitor is a pixel or a photosensitive element of the CCD detector.
利用光刻技术制作掩膜版是通过一系列生产步骤将晶圆表面薄膜的特定部分除去的工艺。在此之后,晶圆表面会留下带有微图形结构的薄膜。通过光刻工艺过程,最终在晶圆上保留的是特征图形部分。在电荷耦合光电探测器5表面设置圆环掩膜板的目的是更加直观的获取接收散射光的各个像素点对应的位置,便于根据各个像素点对应的位置对散射光能量能量的提取,进而快速绘制散射光能量分布图,加快计算所述待测样品的粒度分布的运算速度。The use of photolithography to make a mask is a process in which a specific part of the wafer surface film is removed through a series of production steps. After this, a film with a micropatterned structure remains on the wafer surface. Through the photolithography process, what is finally reserved on the wafer is the characteristic pattern part. The purpose of setting the ring mask on the surface of the charge-coupled photodetector 5 is to more intuitively obtain the corresponding position of each pixel point receiving scattered light, so as to facilitate the extraction of scattered light energy according to the position corresponding to each pixel point, and then quickly Draw a scattered light energy distribution diagram to speed up the operation speed of calculating the particle size distribution of the sample to be tested.
需要指出的是,激光光源1可以根据需求进行选用,如可以为红外光激光光源1或者蓝光激光光源1等,均在保护范围内。It should be pointed out that the laser light source 1 can be selected according to requirements, for example, it can be an infrared laser light source 1 or a blue light laser light source 1, etc., all of which are within the scope of protection.
在上述激光粒度仪的基础上,所述圆环掩膜板包括多个同心圆环10,最小半径圆环的中心与所述电荷耦合光电探测器5的光学中心重合。On the basis of the above-mentioned laser particle size analyzer, the ring mask includes a plurality of concentric rings 10 , and the center of the ring with the smallest radius coincides with the optical center of the charge-coupled photodetector 5 .
如图2所示,圆环掩膜板包括多个同心圆环10,圆环可以为钢环等材质,同心圆环10的数量以及半径不做具体限定,均在保护范围内。As shown in FIG. 2 , the ring mask includes a plurality of concentric rings 10 . The rings can be made of steel rings and other materials. The number and radius of the concentric rings 10 are not specifically limited, and they are all within the scope of protection.
在上述激光粒度仪的基础上,还包括设置于所述激光光源1与所述样品池之间的准直扩束装置2。On the basis of the above-mentioned laser particle size analyzer, it also includes a collimating beam expander 2 arranged between the laser light source 1 and the sample cell.
进一步的,在上述激光粒度仪中,所述准直扩束装置2为开普勒式激光扩束装置,包括会聚透镜7和准直透镜8。Further, in the above-mentioned laser particle size analyzer, the collimating beam expanding device 2 is a Keplerian laser beam expanding device, including a converging lens 7 and a collimating lens 8 .
进一步的,在上述激光粒度仪中,还包括位于所述会聚透镜的焦点处的空间滤波器9。Further, in the above-mentioned laser particle size analyzer, a spatial filter 9 located at the focal point of the converging lens is also included.
一般的激光准直扩束装置2分为两类,开普勒式激光扩束装置和伽利略式激光扩束装置,本实施例优选采用开普勒式激光扩束装置,并在扩束系统的集中焦点处加入了一个空间滤波器9,可以滤掉所有的高阶散射光,通过空间滤波器9的是空间低频的激光束,呈发散光束,再经过准直透镜8后就变成平行单色光束。目的是实现入射到样品池3中的激光束均匀照明,降低杂散光对监测结果的影响,减小系统误差。General laser collimation beam expander 2 is divided into two classes, Kepler type laser beam expander and Galileo type laser beam expander, present embodiment preferably adopts Kepler type laser beam expander, and in the beam expander system A spatial filter 9 is added to the focal point, which can filter out all high-order scattered light. What passes through the spatial filter 9 is a spatially low-frequency laser beam, which is a divergent beam, and then becomes a parallel single beam after passing through the collimating lens 8. colored beams. The purpose is to achieve uniform illumination of the laser beam incident into the sample cell 3, reduce the influence of stray light on the monitoring results, and reduce system errors.
在上述激光粒度仪的基础上,还包括设置于所述样品池3与所述电荷耦合光电探测器5之间的成像透镜4,所述成像透镜4的焦点与所述电荷耦合光电探测器5的中心重合。On the basis of the above-mentioned laser particle size analyzer, it also includes an imaging lens 4 arranged between the sample cell 3 and the charge-coupled photodetector 5, the focal point of the imaging lens 4 is connected to the charge-coupled photodetector 5 centers coincide.
其中,将电荷耦合光电探测器5放置于成像透镜4的焦点处,原因是一部分平行光束被散射,成像透镜4将散射光会聚在其焦平面上,处于焦平面的成像透镜4接收散射光。成像透镜4可以为傅里叶透镜等透镜,根据需要进行选取,均在保护范围内。Wherein, the charge-coupled photodetector 5 is placed at the focal point of the imaging lens 4, because a part of the parallel light beam is scattered, and the imaging lens 4 converges the scattered light on its focal plane, and the imaging lens 4 at the focal plane receives the scattered light. The imaging lens 4 can be a lens such as a Fourier lens, which can be selected according to needs, and all of them are within the scope of protection.
如图3所示,图3为本发明实施例所提供的粒度分布测试方法示意图。As shown in FIG. 3 , FIG. 3 is a schematic diagram of a particle size distribution testing method provided by an embodiment of the present invention.
本发明还包括一种粒度分布测试方法,包括:The present invention also includes a particle size distribution testing method, comprising:
步骤S1:将圆环掩膜板设置于激光粒度仪的电荷耦合光电探测器5上,Step S1: setting the ring mask on the charge-coupled photodetector 5 of the laser particle size analyzer,
步骤S2:激光光源1发射的激光光束通过放有待测样品的样品池3,形成散射光;Step S2: The laser beam emitted by the laser light source 1 passes through the sample cell 3 containing the sample to be tested to form scattered light;
步骤S3:所述电荷耦合光电探测器5接收所述散射光,根据所述圆环掩膜板获取接收所述散射光的像素点的坐标;Step S3: the charge-coupled photodetector 5 receives the scattered light, and obtains the coordinates of the pixel point receiving the scattered light according to the circular mask;
步骤S4:根据所述像素点的坐标绘出所述散射光能量分布图,并计算所述待测样品的粒度分布。Step S4: draw the scattered light energy distribution diagram according to the coordinates of the pixel points, and calculate the particle size distribution of the sample to be tested.
进一步的,在上述粒度分布测试方法中,所述步骤S2之前,还包括:Further, in the above particle size distribution testing method, before the step S2, it also includes:
步骤S11:调整所述圆环掩膜板中最小半径圆环的中心与所述电荷耦合光电探测器5的光学中心重合;Step S11: adjusting the center of the circle with the smallest radius in the circle mask to coincide with the optical center of the charge-coupled photodetector 5;
步骤S12:所述激光光束通过没有所述放置待测样品的所述样品池3,入射至所述电荷耦合光电探测器5上;Step S12: the laser beam is incident on the charge-coupled photodetector 5 through the sample cell 3 without the sample to be measured;
步骤S13:判断所述激光光束在所述电荷耦合光电探测器5上的光斑是否落在所述最小半径圆环的中心,若否,则调整所述激光光束在所述电荷耦合光电探测器5上的对中,若是,则执行所述步骤S2。Step S13: judging whether the spot of the laser beam on the charge-coupled photodetector 5 falls on the center of the circle with the smallest radius, if not, adjusting the laser beam on the charge-coupled photodetector 5 above, if yes, execute the step S2.
其中,将圆环掩模板固定在电荷耦合光电探测器5的表面上,可以通过机械装调的方式完成对激光粒度仪光路在光电探测器上的对中,就是指调整所述激光光束在所述电荷耦合光电探测器5上的光斑是否落在所述最小半径圆环的中心,使得激光粒度仪的光能背景符合测试要求,从而更加直观、清楚地知道电荷耦合光电探测器5上的每一个像素对应的发散光束散射角,进而利用反演算法计算得出粒度分布。Wherein, the ring mask is fixed on the surface of the charge-coupled photodetector 5, and the centering of the optical path of the laser particle size analyzer on the photodetector can be completed through mechanical adjustment, that is, to adjust the laser beam at the surface of the photodetector. Whether the light spot on the charge-coupled photodetector 5 falls on the center of the circular ring with the smallest radius makes the light energy background of the laser particle size analyzer meet the test requirements, so that it is more intuitive and clear to know that each light spot on the charge-coupled photodetector 5 A pixel corresponds to the divergent beam scattering angle, and then the particle size distribution is calculated using an inversion algorithm.
说明书中各个实施例采用递进的方式描述,每个实施例重点说明的都是与其他实施例的不同之处,各个实施例之间相同相似部分互相参见即可。对于实施例公开的装置而言,由于其与实施例公开的方法相对应,所以描述的比较简单,相关之处参见方法部分说明即可。Each embodiment in the description is described in a progressive manner, each embodiment focuses on the difference from other embodiments, and the same and similar parts of each embodiment can be referred to each other. As for the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and for the related part, please refer to the description of the method part.
本文中应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。In this paper, specific examples are used to illustrate the principle and implementation of the present invention, and the descriptions of the above embodiments are only used to help understand the method and core idea of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, some improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
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