WO2021088376A1 - 一种利用散射光的偏振差异测量颗粒折射率的方法及系统 - Google Patents

一种利用散射光的偏振差异测量颗粒折射率的方法及系统 Download PDF

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WO2021088376A1
WO2021088376A1 PCT/CN2020/096495 CN2020096495W WO2021088376A1 WO 2021088376 A1 WO2021088376 A1 WO 2021088376A1 CN 2020096495 W CN2020096495 W CN 2020096495W WO 2021088376 A1 WO2021088376 A1 WO 2021088376A1
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scattered light
refractive index
polarization
particles
particle size
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张福根
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珠海真理光学仪器有限公司
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means
    • G01N15/0211Investigating a scatter or diffraction pattern

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  • the invention relates to the technical field of particle characterization, in particular to a method and system for measuring the refractive index of particles by using the polarization difference of scattered light.
  • Particles refer to geometric bodies with specific shapes generally ranging in size from millimeters to nanometers. Particles not only refer to solid particles, but also fluid particles such as droplets and bubbles. Particles are ubiquitous in nature, and are widely affected or used in industrial production and scientific research. Particle size is one of the most important parameters of particles. In recent years, the application of various new granular materials has placed higher demands on particle size measurement. Laser particle size analyzers based on the principle of static light scattering have been more and more widely used.
  • the scattering light receiving angle of the measuring device (laser particle sizer) is limited to a small angle range, such as 5° or less, the laser particle sizer based on Fraunhofer diffraction theory can be used without input refraction
  • the particle size analysis of the sample is carried out under the condition of low rate; but now the lower limit of the commercial particle size analyzer is as small as 0.1 ⁇ m, so the maximum scattering angle receiving range must reach 60° or more.
  • the scattered light energy distribution of particles of any size is The refractive index is related. If the refractive index of the particles of the same particle size is different, the light energy distribution will have a significant difference. Therefore, when using the laser particle size analyzer based on the Mie scattering theory for particle size analysis, the accurate refractive index of the sample must be input in advance to calculate the corresponding scattering Light energy matrix, and then calculate the particle size distribution according to the scattered light distribution. If the refractive index value entered is wrong, it will lead to wrong analysis results.
  • the refractive index value of the sample is mostly obtained by looking up the table when using the laser particle size analyzer to measure the sample.
  • the refractive index of the actual sample is related to factors such as incident light wavelength and impurity content, so it is difficult to determine the accurate refractive index of the particles, which often leads to large errors between the measurement results of the sample and the actual particle size distribution.
  • the present invention proposes a method and system for measuring the refractive index of particles by using the polarization difference of scattered light.
  • the refractive index and particle size distribution of the measured sample particles are both unknown, only the scattered light signal of the measured particle is used.
  • the refractive index of the particles can be calculated, and then the measured refractive index can be used to obtain an accurate particle size distribution.
  • a method for measuring the refractive index of particles by using the polarization difference of scattered light including the steps:
  • the detector is an array composed of multiple independent detection units, all units are located in the XOZ plane, and each unit corresponds to a different scattering angle. Let the total number of detection units be k.
  • the polarization direction of the scattered light received by each detection unit is perpendicular to the XOZ plane, that is, the scattering surface.
  • are input to the processor.
  • [E d1 ,E d2 ,...,E dk ] T , which is obtained by the calculation of the processor.
  • n (i) set a particle refractive index n (i) , according to Mie theory, calculate the vertical polarization scattering light energy matrix with dimension k ⁇ l And scattered light polarization difference matrix Among them, k is the number of detector units, l is the number of segments representing the particle size of the particles, and i is the number of refractive index values;
  • a system for measuring the refractive index of particles by using the polarization difference of scattered light which is characterized in that it includes a laser light source module, photodetectors arranged in an array, a processor for receiving and processing information from the photodetectors, and storage processing Program memory.
  • the laser light source module includes a linearly polarized light source and a half-wave plate arranged at the exit end of the linearly polarized light source, or the laser light source module includes a natural light source and a polarizer arranged at the exit end of the natural light source.
  • the beneficial effects of the present invention are: when the refractive index and particle size distribution of the measured particle sample are both unknown, the scattered light signal itself obtained by the laser particle size analyzer can be used to obtain the refractive index of the sample, thereby obtaining an accurate particle size distribution of the sample. .
  • Figure 1 is a schematic diagram of the present invention
  • Figure 2 is a schematic diagram of the first laser light source module to realize the optical path
  • Figure 3 is a schematic diagram of the second type of laser light source module to realize the optical path
  • Fig. 4 is a schematic diagram of the optical path realized by the third laser light source module.
  • a method for measuring the refractive index of particles by using the polarization difference of scattered light including the steps:
  • the detector is an array composed of multiple independent detection units, all units are located in the XOZ plane, and each unit corresponds to a different scattering angle. Let the total number of detection units be k.
  • the polarization direction of the scattered light received by each detection unit is perpendicular to the XOZ plane, that is, the scattering surface.
  • are input to the computer.
  • [E d1 ,E d2 ,...,E dk ] T , obtained by computer calculation.
  • the scattered light signal itself obtained by the laser particle size analyzer can be used to calculate the refractive index of the sample, thereby obtaining an accurate particle size distribution of the sample.
  • the measurement system for measuring the refractive index of particles by using the polarization difference of scattered light of this embodiment includes a laser light source module, photodetectors arranged in an array, a processor that receives and processes information from the photodetectors, and a storage processing program Memory.
  • the incident light 1 travels along the Z axis and irradiates the particle 7 located at the origin of the coordinate O (only one is drawn schematically here).
  • Particles in reality, are a group of particles composed of multiple particles of different sizes). After light wave 1 encounters particles 7, it scatters, as shown in the figure, light 2 is scattered.
  • a series of detectors 5 an array composed of multiple independent detectors, each corresponding to a scattering angle 6.
  • the laser particle sizer is placed in the XOZ plane, along the scattering
  • the electric field vector of the scattered light wave propagating on the surface can be decomposed into component 3 that vibrates perpendicular to the XOZ plane (referred to as “vertical polarization component”) and component 4 that vibrates parallel to the XOZ plane (referred to as “horizontal polarization component”).
  • Different detectors are used to receive scattered light with different scattering angles.
  • the vertical polarization components received by each detector are arranged in the order of the detectors from the inside to the outside, respectively denoted as E ⁇ 1 , E ⁇ 2 , ..., E ⁇ k , which are called the distribution of vertically polarized scattered light energy, for simplicity
  • E ⁇ [E ⁇ 1 ,E ⁇ 2 ,...,E ⁇ k ] T
  • k is the total number of independent detection units of the detector.
  • the horizontal component of the scattered light signal is called "horizontal polarization light scatter profile", represented by ⁇
  • [E
  • are input to the computer.
  • the difference between the vertical polarization scattered light energy distribution and the horizontal polarization scattered light energy distribution is called the polarization difference of the scattered light, denoted as E d .
  • E d E ⁇ -E
  • E d is obtained by computer calculation.
  • embodiment can have the following three ways:
  • the laser light source 8 is a linearly polarized light source.
  • the linearly polarized light source is rotated around the Z axis through a rotating mechanism, and the polarization direction of the emitted light is first made parallel to the Y axis. Then the detector 5 measures The scattered light energy distribution is the vertical polarization scattered light distribution E ⁇ . Then, the light source is rotated 90° around the Z axis, and the scattered light energy distribution measured by the detector 5 at this time is the horizontally polarized scattered light energy distribution E
  • the laser light source 8 is linearly polarized light, and the polarization direction is parallel to the Y axis.
  • a half-wave plate 9 is placed on the exit light path, which can rotate around the Z axis.
  • measured scattering detector 5 that is vertically polarized optical energy distribution of scattered optical energy distribution ⁇ ⁇ .
  • the half-wave plate 9 is rotated by 45°.
  • the scattered light energy distribution measured by the detector 5 is the horizontally polarized scattered light energy distribution E
  • the laser light source 8 is non-polarized (natural) light, and a polarizer 10 is placed on the exit light path, which can rotate around the Z axis.
  • the scattered light energy distribution measured by the detector 5 is the vertical polarization scattered light energy distribution E ⁇ .
  • the polarizer is rotated 90°, and the scattered light energy distribution measured by the detector at this time is the horizontally polarized scattered light energy distribution E
  • the memory stores a computer-readable storage medium.
  • the readable storage medium can be various storage media with data storage functions, including but not limited to non-volatile memories such as FIASH and EEPROM.
  • the processor executes the computer During the program, the above-mentioned method for measuring the refractive index of particles can be realized.

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Abstract

一种利用散射光的偏振差异测量颗粒折射率的方法及系统,方法包括获取垂直偏振散射光能分布Ε和水平偏振散射光能分布Ε||,计算散射光能分布偏振差Εd;根据Mie理论,计算一个设定的折射率数值n(i)下的维数为k×l的垂直偏振散射光能矩阵(aa)和散射光偏振差矩阵(bb)计算被测颗粒的粒度分布W(i),获取散射光的偏振差(cc),计算Ε d与(cc)的均方差σ(i),改变折射率的数值,重复上述过程,获得均方差最小的折射率,就是颗粒的真实折射率,使用此折射率计算的粒度分布即为颗粒真实的粒度分布。一种实现该方法的系统,在被测颗粒样品的折射率与粒度分布均未知的情况下,可利用激光粒度仪获得的散射光信号本身,求出样品的折射率,进而获得准确的样品粒度分布。

Description

一种利用散射光的偏振差异测量颗粒折射率的方法及系统 技术领域
本发明涉及颗粒表征技术领域,具体涉及一种利用散射光的偏振差测量颗粒折射率的方法及系统。
背景技术
颗粒是指尺寸一般在毫米到纳米之间具有特定形状的几何体,颗粒不仅指固体颗粒,还包括雾滴、气泡等流体颗粒。颗粒在自然界中无处不在,且广泛影响或应用于工业生产和科学研究。颗粒大小是颗粒的最重要的参数之一。近年来各种新型颗粒材料的应用,对颗粒粒径测量有了更高要求。基于静态光散射原理的激光粒度仪得到了越来越广泛的应用。
根据光散射的几何光学近似理论,颗粒直径远大于光波长时在小角范围内其散射光强以衍射光为主,其光能分布主峰出现在前向小角度内。如果只测量远大于光波长的颗粒且测量装置(激光粒度仪)的散射光接收角限制在小角范围内,例如5°以下,那么基于夫琅禾费衍射理论的激光粒度仪可以在不输入折射率的条件下对样品进行粒度分析;但现在商品化的粒度仪测量下限小至0.1μm,为此最大散射角接收范围要达到60°以上,此时任何大小的颗粒的散射光能分布都与折射率有关,相同粒径的颗粒如果折射率不同,光能分布具有明显差异,故在使用基于Mie散射理论的激光粒度仪进行粒度分析时,需提前输入样品准确的折射率,计算相应的散射光能矩阵,然后根据散射光分布反演计算粒度分布。如果输入的折射率数值是错误的,则将导致错误的分析结果。
目前使用激光粒度仪测样时样品折射率值多为查表获得。但是实际样品折射率与入射光波长和杂质含量等因素有关,故很难确定颗粒的准确折射率, 这常导致样品的测量结果与实际粒度分布有较大误差。
到目前为止,虽然已经有几种利用散射光信号测量折射率的方法,但都存在这样那样的局限。
发明内容
为了克服以上问题,本发明提出一种利用散射光的偏振差测量颗粒折射率的方法及系统,在被测样品颗粒的折射率和粒度分布均未知的情况下,仅仅利用被测颗粒散射光信号本身,就能计算颗粒的折射率,再利用测得的折射率得出准确的粒度分布。
本发明的技术方案为:
一种利用散射光的偏振差异测量颗粒折射率的方法,包括步骤:
S1,当光波沿Z轴照射到位于坐标原点O的颗粒,被颗粒散射的光被位于XOZ平面的探测器所接收。所述探测器是由多个独立探测单元组成的阵列,所有单元都位于XOZ平面内,每个单元对应不同的散射角。设探测单元总数为k个。当照明光为线偏振光,且偏振方向平行于Y轴时,各探测单元接收到的散射光的偏振方向均垂直于XOZ平面,即散射面。按散射角的大小从里往外排序,记各探测单元接收到的光能分别为E ⊥1,E ⊥2,…,E ⊥k,用矢量E =[E ⊥1,E ⊥2,…,E ⊥k] T表示,称为垂直偏振的散射光能分布。类似地,用偏振方向平行于X轴的线偏振光照明颗粒时,探测器各单元接收到的光能就组成水平偏振的散射光能分布,用E ||表示,E ||=[E ||1,E ||2,…,E ||k] T。E 和E ||输入至处理器。把垂直偏振散射光能分布和水平偏振散射光能分布之差称为散射光能分布的偏振差,记为E d。故E d=E -E ||=[E d1,E d2,…,E dk] T,通过处理器的计算获得。
S2,设定一个颗粒折射率n (i),根据Mie理论,计算维数为k×l的垂直偏 振散射光能矩阵
Figure PCTCN2020096495-appb-000001
和散射光偏振差矩阵
Figure PCTCN2020096495-appb-000002
其中,k为探测器单元的个数,l为颗粒的代表粒径的分段数,i为折射率取值编号;
S3,根据获得的Ε 数值和垂直偏振的散射光能矩阵
Figure PCTCN2020096495-appb-000003
反演计算被测颗粒的粒度分布
Figure PCTCN2020096495-appb-000004
其中,
Figure PCTCN2020096495-appb-000005
表示假设折射率为n (i)时,反演计算得到的粒径处于第j个代表粒径段内的颗粒体积与颗粒总体积的比值;
S4,根据S3所得的粒度分布W (i)和散射光偏振差矩阵
Figure PCTCN2020096495-appb-000006
获取散射光的偏振差分布
Figure PCTCN2020096495-appb-000007
S5,根据散射光偏振差E d
Figure PCTCN2020096495-appb-000008
得到均方差
Figure PCTCN2020096495-appb-000009
S6,将颗粒折射率变为n (j),重复步骤2-5,计算均方差σ (j),如此往复,找到均方差最小时对应的颗粒折射率即为颗粒的真实折射率,该折射率对应的粒度分布即为真实的粒度分布。
一种利用散射光的偏振差测量颗粒折射率的系统,其特征在于:包括激光光源模组、成阵列式排布的光电探测器和接收并处理来自光电探测器信息的处理器、及存储处理程序的存储器。
进一步地,所述激光光源模组包括线偏振光光源及设置在线偏振光光源出射端的半波片,或者所述激光光源模组包括自然光光源及设置在自然光光源出射端的起偏器。
本发明的有益效果为:在被测颗粒样品的折射率和粒度分布均未知的情况下,可利用激光粒度仪获得的散射光信号本身,求出样品的折射率,进而获得准确的样品粒度分布。
附图说明
图1为本发明的原理图;
图2为第一种激光光源模组实现光路示意图;
图3为第二种激光光源模组实现光路示意图;
图4为第三种激光光源模组实现光路示意图。
具体实施方式
一种利用散射光的偏振差异测量颗粒折射率的方法,包括步骤:
S1,当光波沿Z轴照射到位于坐标原点O的颗粒,被颗粒散射的光被位于XOZ平面的探测器所接收。所述探测器是由多个独立探测单元组成的阵列,所有单元都位于XOZ平面内,每个单元对应不同的散射角。设探测单元总数为k个。当照明光为线偏振光,且偏振方向平行于Y轴时,各探测单元接收到的散射光的偏振方向均垂直于XOZ平面,即散射面。按散射角的大小从里往外排序,记各探测单元接收到的光能分别为E ⊥1,E ⊥2,…,E ⊥k,用矢量E =[E ⊥1,E ⊥2,…,E ⊥k] T表示,称为垂直偏振的散射光能分布。类似地,用偏振方向平行于X轴的线偏振光照明颗粒时,探测器各单元接收到的光能就组成水平偏振的散射光能分布,用表示E ||,E ||=[E ||1,E ||2,…,E ||k] T。E 和E ||输入至计算机。把垂直偏振散射光能分布和水平偏振散射光能分布之差称为散射光能分布的偏振差,记为E d。故E d=E -E ||=[E d1,E d2,…,E dk] T,通过计算机的计算获得。
S2,假设一个颗粒折射率n (i),根据Mie理论,计算维数为k×l的垂直偏振散射光能矩阵
Figure PCTCN2020096495-appb-000010
和散射光偏振差矩阵
Figure PCTCN2020096495-appb-000011
其中,k为探测器单元的个数,l为颗粒的代表粒径的分段数,i为折射率取值编号;
S3,根据获得的Ε 数值和垂直偏振的散射光能矩阵
Figure PCTCN2020096495-appb-000012
反演计算被测 颗粒的粒度分布
Figure PCTCN2020096495-appb-000013
其中,
Figure PCTCN2020096495-appb-000014
表示假设折射率为n (i)时,反演计算得到的粒径处于第j个代表粒径段内的颗粒体积与颗粒总体积的比值;
S4,根据S3所得的粒度分布W (i)和散射光偏振差矩阵
Figure PCTCN2020096495-appb-000015
获取散射光的偏振差分布
Figure PCTCN2020096495-appb-000016
S5,根据散射光偏振差E d
Figure PCTCN2020096495-appb-000017
得到均方差
Figure PCTCN2020096495-appb-000018
S6,将颗粒折射率变为n (j),重复步骤2-5,计算均方差σ (j)。如此往复,找到均方差最小时对应的颗粒折射率即为颗粒的真实折射率,该折射率对应的粒度分布即为真实的粒度分布。
通过本实施例提供的方法,在被测颗粒样品的折射率未知的情况下,可利用激光粒度仪获得的散射光信号本身,求出样品的折射率,进而获得准确的样品粒度分布。
本实施例的利用散射光的偏振差测量颗粒折射率的测量系统包括激光光源模组、成阵列式排布的光电探测器和接收并处理来自光电探测器的信息的处理器、及存储处理程序的存储器。
使用激光粒度仪测量被测样品的散射光能,具体的,如图1所示,入射光1沿着Z轴传播,照射到位于坐标原点O的颗粒7(此处只示意性地画了一个颗粒,现实情况下是多个不同大小颗粒组成的颗粒群)上。光波1遇到颗粒7后,发生散射,如图中散射光线2。激光粒度仪中的一系列探测器5(是多个独立探测器组成的阵列,每个探测器都对应一个散射角6。此处只示意性地画了一个)置于XOZ平面内,沿散射面传播的散射光波的电场矢量可以分 解为垂直于XOZ平面振动的分量3(称为“垂直偏振分量”)和平行于XOZ平面振动的分量4(称为“水平偏振分量”)。不同的探测器用于接收不同散射角的散射光。各个探测器接收到的垂直偏振分量按探测器从里到外排布的顺序,分别记为E ⊥1,E ⊥2,…,E ⊥k,称为垂直偏振的散射光能分布,为简洁起见,用矢量E 表示,即E =[E ⊥1,E ⊥2,…,E ⊥k] T,此处k为探测器独立探测单元的总个数。类似地,这些散射光信号的水平分量称为“水平偏振散射光能分布”,用Ε ||表示,E ||=[E ||1,E ||2,…,E ||k] T。E 和E ||输入至计算机。把垂直偏振散射光能分布和水平偏振散射光能分布之差称为散射光的偏振差,记为E d。故E d=E -E ||。E d通过计算机的计算获得。
本实施例的垂直偏振散射光能分布Ε 和水平偏振散射光能分布Ε ||可有以下三种实施方式实现:
一:如图2所示,激光光源8为线偏振光光源,通过转动机构将线偏振光光源绕Z轴转动,先使出射光的偏振方向平行于Y轴,这时探测器5测得的散射光能分布即为垂直偏振散射光分布Ε 。然后将光源绕Z轴转动90°,此时探测器5测得的散射光能分布即为水平偏振散射光能分布Ε ||
二:如图3所示,激光光源8为线偏振光,且偏振方向平行于Y轴。在出射光路上放置一个半波片9,它可绕Z轴转动。当半波片9的主截面平行于Y轴时,探测器5测得的散射光能分布即为垂直偏振散射光能分布Ε 。然后将半波片9转动45°,此时探测器5测得的散射光能分布即为水平偏振散射光能分布Ε ||
三:如图4所示,激光光源8为非偏振(自然)光,在出射光路上放置起偏器10,它可绕Z轴转动。当起偏器10的起偏方向平行于Y轴时,探测器5测得的散射光能分布即为垂直偏振散射光能分布Ε 。然后将起偏器转动 90°,此时探测器测得的散射光能分布即为水平偏振散射光能分布Ε ||
还需要说明的是,存储器存储有计算机可读存储介质,可读存储介质可以是具有数据存储功能的各种存储介质,包括但不限于FIASH、EEPROM等非易失性存储器,当处理器执行计算机程序时,可以实现上述的颗粒折射率的测量方法。
以上所属实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制,应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此本发明专利的保护范围应以所附权利要求为准。

Claims (6)

  1. 一种利用散射光的偏振差异测量颗粒折射率的方法,其特征在于,包括步骤:
    S1,分别获取光波照射到位于坐标原点O的颗粒样品上后产生的垂直偏振散射光能分布E =[E ⊥1,E ⊥2,…,E ⊥k] T和水平偏振散射光能分布E ||=[E ||1,E ||2,…,E ||k] T,计算散射光的偏振差E d=E -E ||=[E d1,E d2,…,E dk] T
    S2,根据Mie理论,计算在颗粒的折射率n (i)下的维数为k×l的垂直偏振散射光能矩阵
    Figure PCTCN2020096495-appb-100001
    和散射光偏振差矩阵
    Figure PCTCN2020096495-appb-100002
    其中,k为探测光能的探测器单元的个数,l为颗粒的代表粒径的分段数,i为折射率取值编号;
    S3,根据获得的Ε 数值和垂直偏振的散射光能矩阵
    Figure PCTCN2020096495-appb-100003
    反演计算被测颗粒的粒度分布
    Figure PCTCN2020096495-appb-100004
    其中,
    Figure PCTCN2020096495-appb-100005
    表示假设折射率为n (i)时,反演计算得到的粒径处于第j个代表粒径段内的颗粒体积与颗粒总体积的比值;
    S4,根据粒度分布W (i)和散射光偏振差矩阵
    Figure PCTCN2020096495-appb-100006
    获取散射光的偏振差分布
    Figure PCTCN2020096495-appb-100007
    S5,根据散射光偏振差E d
    Figure PCTCN2020096495-appb-100008
    得到均方差
    Figure PCTCN2020096495-appb-100009
    S6,将S2中的颗粒折射率变为n (j),重复步骤2-5,计算均方差σ (j)。找到均方差最小时对应的折射率即为颗粒的真实折射率,该折射率对应的粒度分布即为真实的粒度分布。
  2. 如权利要求1所述的散射光的偏振差异测量颗粒折射率的方法,其特征在于,S2中散射光偏振差矩阵
    Figure PCTCN2020096495-appb-100010
    由垂直偏振散射光能矩阵
    Figure PCTCN2020096495-appb-100011
    和水平 偏振散射光能矩阵
    Figure PCTCN2020096495-appb-100012
    之差获得,即
    Figure PCTCN2020096495-appb-100013
  3. 如权利要求1所述的散射光的偏振差异测量颗粒折射率的方法,其特征在于,所述S1中垂直偏振散射光能分布Ε 和水平偏振散射光能分布Ε ||分别由成阵列式排布的激光探测器获得。
  4. 一种利用散射光的偏振差异测量颗粒折射率的系统,其特征在于:包括激光光源模组、成阵列式排布的多个光电探测器和接收并处理探测器输出的电信号的处理器、及存储处理程序的存储器。
  5. 如权利要求4所述的利用散射光的偏振差异测量颗粒折射率的系统,其特征在于:所述激光光源模组包括线偏振激光光源及光源旋转装置,或线偏振光光源与设置在线偏振光光源出射端的可旋转45°或以上的半波片。
  6. 如权利要求4所述的利用散射光的偏振差异测量颗粒折射率的系统,其特征在于:所述激光光源模组包括非偏振激光光源及设置在光源出射端的可旋转90°或以上的起偏器。
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