Raman spectrum analysis system and method for particle moisture bonding strength and content

Abstract

The invention discloses a Raman spectrum analysis system and method for particle moisture bonding strength and content, and the system comprises a laser generation module which is used for generating laser; the surface light source light path is used for adjusting the laser to form a surface light source and guiding light of the surface light source to a to-be-detected sample area; the point light source light path is used for adjusting the laser to form a point light source and guiding the light of the point light source to a to-be-detected sample area; the mobile scanning detection assembly is used for placing a to-be-detected sample and adjusting the detected position of the to-be-detected sample; and the Raman spectrum assembly is used for receiving Raman signals excited by the surface light source and the point light source and carrying out conjoint analysis on field signals and point signals to obtain the surface moisture binding degree and distribution of the sample to be detected. The system and the method provided by the invention can realize detection and analysis of the particle moisture molecule binding state and content.

Description

Technical Field

[0001] The invention relates to the field of granular medium physical and chemical property testing, and in particular to a Raman spectroscopy analysis system and method for granular water binding strength and content. Background Art

[0002] In many discrete media systems, the complex interaction between particles and water often makes the physical and chemical properties of substances unique. Taking natural soil as an example, water in soil can be divided into different types such as mineral component water, bound water, liquid water, gaseous water, and solid water according to the existence form, state, activity and interaction of water with soil. The content of each type is the main factor determining the properties of water.

[0003] In the development and application of particle-related engineering technologies, obtaining information on the water binding state and water content in particle media is of great significance for the prediction of the macroscopic properties of the medium and the parameter design of related process flows. At the micro-nano scale of the particle surface interface, obtaining the distribution of various types of water on the surface of the particle plays an important supporting role in the research and development of particle technology, the revelation of microscopic mechanisms, and the active regulation and design of particle behavior.

[0004] At present, the detection of different types of water on the surface of particles at home and abroad is mainly achieved indirectly based on the differences in boiling points, freezing points and salt content of different types of water. Usually, only part of the water content can be obtained, and the accuracy of the test results depends on the accuracy of the experimental testing methods. There is a lack of rapid, accurate and comprehensive methods and equipment for analyzing the water binding state and distribution on the particle surface.

[0005] Spectroscopic technology is the most effective experimental method to study the occurrence form of water molecules. It can determine the difference in the combination form of water and solid by distinguishing the vibration frequency of water molecules or the radial distribution difference of oxygen and hydrogen atoms. Combined with spectral analysis, it can effectively classify the water binding type and make quantitative distinctions, so as to accurately obtain the water binding state and content of particles. Therefore, the rapid, accurate and comprehensive research on the detection and analysis technology of the degree and distribution of water binding on the particle surface plays an important supporting role in the development of cutting-edge particle technology.

[0006] In view of the above shortcomings, the present invention urgently needs to provide a Raman spectroscopy analysis system and method for particle moisture binding strength and content, so as to solve the technical problems that traditional particle moisture detection methods are difficult to quickly, accurately and conveniently test the particle surface moisture binding strength and content. Summary of the invention

[0007] The technical problem to be solved by the present invention is to provide a Raman spectroscopy analysis system and method for particle water binding strength and content in view of the defects in the prior art.

[0008] The technical solution adopted by the present invention to solve its technical problem is:

[0009] The present invention provides a Raman spectroscopy analysis system for particle water binding strength and content, the system comprising:

[0010] A laser generating module, used for generating laser;

[0011] A surface light source optical path, used to adjust the laser to form a surface light source, and guide the light of the surface light source to the sample area to be detected;

[0012] A point light source optical path, used to adjust the laser to form a point light source, and guide the light of the point light source to the sample area to be detected;

[0013] A mobile scanning and detection component is used to place the sample to be detected and adjust the detected position of the sample to be detected;

[0014] The Raman spectroscopy component is used to receive the Raman signals excited by the surface light source and the point light source, and perform a joint analysis of the field signal and the point signal to obtain the degree of water binding and distribution on the surface of the sample to be detected.

[0015] Furthermore, the Raman spectroscopy component of the present invention comprises:

[0016] A field information receiving channel, used for receiving the Raman signal excited by the surface light source;

[0017] A point information receiving channel, used for receiving the Raman signal excited by the point light source;

[0018] A Raman spectrometer connected to the output ends of the field information receiving channel and the point information receiving channel, and used for converting the Raman signal excited by the surface light source and the Raman signal excited by the point light source into an electrical signal;

[0019] A field-point information joint analysis module is connected to the output end of the Raman spectrometer and is used to generate a Raman spectrum of the sample to be detected according to the electrical signal to obtain the water binding degree and distribution on the surface of the sample to be detected;

[0020] The control module is connected to the field-point information joint analysis module and the mobile scanning and detection component, and is used to control the mobile scanning and detection component.

[0021] Furthermore, the mobile scanning and detection component of the present invention comprises:

[0022] A three-dimensional motion control console, used to change the position of the test sample in three-dimensional space;

[0023] The focus detection and control optical control module is connected to both the field information receiving channel and the point information receiving channel, and is used to adjust the position of the focal plane or focus in three-dimensional space.

[0024] Furthermore, the implementation of the surface light source light path and the point light source light path of the present invention includes:

[0025] Two optical paths with independent spatial positions;

[0026] Alternatively, a switchable optical path can be constructed by adding light-transmitting components with different apertures to a common optical path.

[0027] Furthermore, the implementation of the field signal receiving channel and the point signal receiving optical path of the present invention includes:

[0028] Signal transmission channels with independent spatial locations;

[0029] Alternatively, a switchable signal transmission channel is constructed by adding a pinhole light-transmitting structure to the imaging plane of the common signal transmission channel.

[0030] Furthermore, the samples to be tested in the present invention are water-containing particles including rock particles and sludge particles.

[0031] The present invention provides a Raman spectroscopy analysis method for particle moisture binding strength and content, using the Raman spectroscopy analysis system for particle moisture binding strength and content, the method comprises the following steps:

[0032] Step 1: Place the sample to be tested on a three-dimensional motion console, and the laser generating module emits laser;

[0033] Step 2: Point light source optical path: The laser is adjusted to form a point light source, and the light of the point light source is guided to the sample area to be detected. The detection focus optical control module focuses the light of the point light source on the surface of the sample to be detected. The point information receiving channel receives the Raman signal excited by the point light source, and the Raman spectrometer converts the Raman signal into an electrical signal. By adjusting the focus position and the three-dimensional motion console, the focus position P x,y,z Move in the z-axis direction to obtain different Raman spectral signals; extract the peak frequency f of each measurement point through the field-point information joint analysis module z And arrange them in order of z coordinates, and take the frequency value f where the adjacent frequency difference is greater than the threshold N i Form the basis vector t, the different frequency values ​​f of the basis vector i Represents different types of water;

[0034] Step 3: The surface light source optical path adjusts the laser to form a surface light source, and guides the surface light source light to the sample area to be detected. The detection focus optical control module focuses the surface light source light on the surface of the sample to be detected. The field information receiving channel receives the Raman signal excited by the surface light source, and the Raman spectrometer converts the Raman signal into an electrical signal. The Raman spectrum is analyzed by the field-point information joint analysis module with the characteristic frequency value f in the basis vector t. i Decompose and use Gaussian function to fit the curve, and then get the water content of each combination type;

[0035] Step 4: According to the characteristic frequency peak f i and different characteristic frequency peaks f i Gaussian decomposition peak area A i Calculate the field average spectral weighted peak frequency and define the average moisture consolidation degree χ w represents the average bonding strength between water and solid, and substitutes each characteristic peak frequency f i Get the degree of consolidation corresponding to the moisture type.

[0036] Furthermore, the method for obtaining the content of water of each combination type in the method of the present invention is specifically as follows:

[0037] The Raman spectrum is calculated by taking the characteristic frequency value f in the basis vector t i Decompose and use Gaussian function for curve fitting:

[0038] ∫ L H fdx=∑f i ·A i

[0039] In the formula, A i are different characteristic frequency peaks f i Gaussian decomposition peak area, the water content of each binding type x i It is expressed as:

[0040]

[0041] Furthermore, the specific method of the solidification degree corresponding to the moisture type in the method of the present invention is:

[0042] Calculate the field average spectral weighted peak frequency F w :

[0043]

[0044] Define the average degree of moisture consolidation χ w Represents the average bonding strength between water and solid:

[0045]

[0046] In the formula, F WS Represents the characteristic peak frequency of ice. For solid water such as ice, the water binding degree is 1; f 0 It represents the characteristic peak frequency corresponding to free water when the binding strength between water and solid is the lowest. It is usually the frequency farthest from F in the measured Raman signal. WS Peak frequency f on one side i The extreme value of .

[0047] Calculate the frequency f of each characteristic peak i Degree of consolidation corresponding to moisture type:

[0048]

[0049] For χ i The greater the moisture content, the higher the degree of consolidation.

[0050] Furthermore, in the method of the present invention, a point light source Raman spectrum signal of the degree of binding between water molecules and solid particles is obtained by a point light source optical path, and the peak frequency information of water molecules reflecting the degree of binding between water molecules and solid particles is extracted, and the water molecule binding state information is contained in the peak frequency of the spectrum; a field light source Raman spectrum signal of the degree of binding between water molecules and solid particles is obtained by a field light source optical path, and different types of moisture contents are obtained by inverting the field Raman spectrum signal.

[0051] The beneficial effects produced by the present invention are:

[0052] 1. The present invention provides a Raman spectroscopy analysis system and method for particle moisture binding strength and content, which solves the technical problems that traditional particle moisture detection methods are difficult to quickly, accurately and conveniently test the particle surface moisture binding strength and content.

[0053] 2. The system of the present invention adopts a two-path design of a point light source optical path and a surface light source optical path, which can obtain point light source Raman spectral signals and surface light source Raman spectral signals. By processing their signals, more comprehensive particle moisture binding strength and content analysis results can be obtained; the position of the sample to be tested can be precisely controlled through a three-dimensional motion control console, and multiple groups of experimental data can be collected; through the detection foot pad optical control module, the focus of the two laser paths of the point light source and the surface light source can be accurately adjusted.

[0054] 3. The present invention provides a Raman spectroscopy detection and analysis method for particle moisture distribution, which can detect and analyze the binding state and content of particle moisture molecules.

[0055] 4. In the method of the present invention, the difference in the combination form of water and solid is judged by distinguishing the vibration frequency of water molecules or the difference in the radial distribution of oxygen and hydrogen atoms. Combined with spectral analysis, the water combination type can be effectively classified and quantitatively distinguished.

[0056] 5. The method of the present invention adopts a dual-light path Raman system of a surface light source and a point light source to realize the classification of moisture types on the particle surface and the quantitative analysis of the proportion of each type of moisture. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] The present invention will be further described below with reference to the accompanying drawings and embodiments, in which:

[0058] Figure 1 The Raman spectroscopy analysis system and method for the particle moisture binding strength and content of the present invention is a schematic diagram;

[0059] Figure 2 This is a diagram showing an implementation scheme of a Raman spectroscopy analysis system and method for particle moisture binding strength and content according to the present invention. DETAILED DESCRIPTION

[0060] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0061] Example 1

[0062] The embodiment of the present invention provides a Raman spectroscopy analysis system and method for particle water binding strength and content, and its design principle is as follows:

[0063] The information about the binding state of water molecules and solids is contained in the peak frequency of the spectrum: on the surface of particles, water molecules are bound by the particles, which inhibits the symmetrical stretching of the OH bonds of water molecules, resulting in a "red-shifted frequency". Therefore, a higher peak frequency corresponds to a higher frequency vibration of water molecules, and water molecules that are more tightly bound to solids will exhibit a lower spectral peak frequency.

[0064] The OH vibration frequency of a water molecule is not only related to the hydrogen bonding state formed by the water molecule, but also to the hydrogen bonding state of other water molecules around the water molecule. The field average spectrum peak frequency is the result of the superposition of all vibration frequencies of the OH bonds. The width of the Raman spectrum reflects the diversity of the OH vibration forms of water molecules. The wider the spectrum, the more types of water molecules there are.

[0065] By distinguishing the vibration frequency of water molecules or the radial distribution difference of oxygen and hydrogen atoms, the difference in the binding form of water and solid can be judged. Combined with spectral analysis, the water binding types can be effectively classified and quantitatively distinguished, thereby accurately obtaining the water binding state and content of particles. A Raman spectroscopy analysis system and method for particle water binding strength and content are given.

[0066] Example 2

[0067] Based on the design principle of Example 1, the present invention provides a Raman spectroscopy analysis system for particle water binding strength and content. Figure 1 As shown, the system includes:

[0068] A laser generating module 33, used for generating laser;

[0069] The surface light source optical path 31 is used to adjust the laser to form a surface light source and guide the light of the surface light source to the sample area to be detected;

[0070] Point light source optical path 32, used to adjust the laser to form a point light source, and guide the light of the point light source to the sample area to be detected;

[0071] A mobile scanning detection component 2, used for adjusting the detection position of the sample 22 to be detected;

[0072] The Raman spectroscopy component 1 is used to receive the Raman signals excited by the surface light source and the point light source, and perform a joint analysis of the field signal and the point signal to obtain the degree and distribution of water binding on the surface of the sample to be detected.

[0073] A field information receiving channel 14, used for receiving the Raman signal excited by the surface light source;

[0074] A point information receiving channel 15, used for receiving the Raman signal excited by the point light source;

[0075] A Raman spectrometer 13, used for converting the Raman signal into an electrical signal;

[0076] The field-point information joint analysis module 12 is used to generate a Raman spectrum of the sample to be detected 22 according to the electrical signal, and obtain the water binding degree and distribution on the surface of the sample to be detected;

[0077] The control module 11 is used to control the mobile scanning and detecting component 2 .

[0078] A three-dimensional motion control console 21, used to change the position of the test sample 22 in three-dimensional space;

[0079] The focus detection and control optical control module 23 is used to adjust the position of the focal plane or the focus in three-dimensional space.

[0080] In a preferred embodiment of the present invention, the surface light source optical path 31 and the point light source optical path 32 may be two optical paths with independent spatial positions, or may be switchable optical paths constructed by adding light-transmitting components with different apertures to a common optical path.

[0081] In a preferred embodiment of the present invention, the field signal receiving channel 14 and the point signal receiving optical path 15 can be signal transmission channels with independent spatial positions, or can be switchable signal transmission channels constructed by adding a pinhole light-transmitting structure to the imaging plane of the common signal transmission channel.

[0082] In a preferred embodiment of the present invention, the Raman spectroscopy detection and analysis system for particle moisture distribution can be used to detect samples 22 to be detected, such as rock particles, sludge particles, and other water-containing particles;

[0083] Example 3

[0084] The embodiment of the present invention provides a Raman spectrum detection and analysis method for particle moisture distribution based on the design principle of embodiment 1 and the system of embodiment 2. The method includes the following steps:

[0085] Step 1, the laser generating module 33 generates laser;

[0086] Step 2: The point light source optical path 32 adjusts the laser to form a point light source, and guides the point light source light to the sample area to be detected. The detection focus optical control module 23 focuses the point light source light on the surface of the sample to be detected 22. The point information receiving channel 15 receives the Raman signal excited by the point light source, and the Raman spectrometer 13 converts the Raman signal into an electrical signal. By adjusting the focus position and the three-dimensional motion console 21, the focus position P x,y,z Move in the z-axis direction to obtain different Raman spectrum signals and extract the peak frequency f at each measurement point z And arrange them in order of z coordinates, and take the frequency value f where the adjacent frequency difference is greater than the threshold N i Form the basis vector t, the different frequency values ​​f of the basis vector i Represents different types of water.

[0087] Step 3: The surface light source optical path 31 adjusts the laser to form a surface light source, and guides the surface light source light to the sample area to be detected. The detection focus optical control module 23 focuses the surface light source light on the surface of the sample to be detected 22. The field information receiving channel 14 receives the Raman signal excited by the surface light source, and the Raman spectrometer 13 converts the Raman signal into an electrical signal. The Raman spectrum is calculated by taking the characteristic frequency value f in the basis vector t as the input. i Decompose and use Gaussian function for curve fitting:

[0088] ∫ L H fdx=∑f i ·A i

[0089] In the formula, A i are different characteristic frequency peaks f iGaussian decomposition peak area. Calculate the content of water x of different binding types i for:

[0090]

[0091] Calculate the field average spectral weighted peak frequency F w :

[0092]

[0093] Define the average degree of moisture consolidation χ w Represents the average bonding strength between water and solid:

[0094]

[0095] In the formula, F WS Represents the characteristic peak frequency of ice. For solid water such as ice, the water binding degree is 1; f 0 It represents the characteristic peak frequency corresponding to free water when the binding strength between water and solid is the lowest. It is usually the frequency farthest from F in the measured Raman signal. WS Peak frequency f on one side i Calculate the frequency f of each characteristic peak i Degree of consolidation corresponding to moisture type:

[0096]

[0097] For χ i The greater the moisture content, the higher the degree of consolidation.

[0098] In summary, the present invention can effectively classify and quantitatively distinguish the water binding types by distinguishing the vibration frequency of water molecules or the radial distribution difference of oxygen and hydrogen atoms to determine the difference in the binding forms of water and solids, combined with spectral analysis methods;

[0099] The present invention adopts a double-light-path Raman system of a surface light source and a point light source to realize the classification of moisture types on the particle surface and the quantitative analysis of the proportion of each type of moisture.

[0100] It should be understood that the size of the serial numbers of the steps in the above embodiments does not mean the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.

[0101] It should be understood that those skilled in the art can make improvements or changes based on the above description, and all these improvements and changes should fall within the scope of protection of the appended claims of the present invention.

Claims

1. A Raman spectroscopy analysis system for particle water binding strength and content, characterized in that: The system includes: A laser generating module (33), used for generating laser; A surface light source optical path (31), used for adjusting the laser to form a surface light source, and guiding the light of the surface light source to a sample area to be detected; A point light source optical path (32), used for adjusting the laser to form a point light source, and guiding the light of the point light source to a sample area to be detected; A mobile scanning detection component (2) is used to place a sample to be detected (22) and adjust the detected position of the sample to be detected (22); The Raman spectroscopy component (1) is used to receive the Raman signals excited by the surface light source and the point light source, and to perform a joint analysis of the field signal and the point signal to obtain the degree of water binding and distribution on the surface of the sample to be detected (22).

2. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 1, characterized in that: The Raman spectroscopy component (1) comprises: A field information receiving channel (14), used for receiving the Raman signal excited by the surface light source; A point information receiving channel (15), used for receiving the Raman signal excited by the point light source; A Raman spectrometer (13), connected to the output ends of the field information receiving channel (14) and the point information receiving channel (15), for converting the Raman signal excited by the surface light source and the Raman signal excited by the point light source into an electrical signal; A field-point information joint analysis module (12) is connected to the output end of the Raman spectrometer (13) and is used to generate a Raman spectrum of the sample to be detected (22) according to the electrical signal to obtain the water binding degree and distribution on the surface of the sample to be detected (22); The control module (11) is connected to the field-point information joint analysis module (12) and the mobile scanning detection component (2), and is used to control the mobile scanning detection component (2).

3. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 2, characterized in that: The mobile scanning and detection component (2) comprises: A three-dimensional motion control console (21) for changing the position of the detection sample (22) in three-dimensional space; The focus detection control optical control module (23) is connected to both the field information receiving channel (14) and the point information receiving channel (15) and is used to adjust the position of the focal plane or focus in three-dimensional space.

4. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 1, characterized in that: The implementation method of the surface light source optical path (31) and the point light source optical path (32) includes: Two optical paths with independent spatial positions; Alternatively, a switchable optical path can be constructed by adding light-transmitting components with different apertures to a common optical path.

5. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 1, characterized in that: The implementation method of the field signal receiving channel (14) and the point signal receiving optical path (15) includes: Signal transmission channels with independent spatial locations; Alternatively, a switchable signal transmission channel is constructed by adding a pinhole light-transmitting structure to the imaging plane of the common signal transmission channel.

6. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 1, characterized in that: The samples (22) to be tested are water-containing particles including rock particles and sludge particles.

7. A Raman spectroscopy analysis method for particle moisture binding strength and content, using the Raman spectroscopy analysis system for particle moisture binding strength and content according to any one of claims 1 to 6, characterized in that: The method comprises the following steps: Step 1: placing a sample to be tested (22) on a three-dimensional motion control console (21), and emitting laser light from a laser generating module (33); Step 2, point light source optical path (32) adjusts the laser to form a point light source, and guides the light of the point light source to the area of ​​the sample to be detected (22), the detection focus optical control module (23) focuses the light of the point light source on the surface of the sample to be detected (22), the point information receiving channel (15) receives the Raman signal excited by the point light source, and the Raman spectrometer (13) converts the Raman signal into an electrical signal; by adjusting the focus position and the three-dimensional motion control console (21), the focus position P x,y,z Move in the z-axis direction to obtain different Raman spectrum signals; extract the peak frequency f of each measurement point through the field-point information joint analysis module (12) z And arrange them in order of z coordinates, and take the frequency value f where the adjacent frequency difference is greater than the threshold N i Form the basis vector t, the different frequency values ​​f of the basis vector i Represents different types of water; Step 3: The surface light source optical path (31) adjusts the laser to form a surface light source, and guides the surface light source light to the area of ​​the sample to be detected (22); the detection focus optical control module (23) focuses the surface light source light on the surface of the sample to be detected (22); the field information receiving channel (14) receives the Raman signal excited by the surface light source, and the Raman spectrometer (13) converts the Raman signal into an electrical signal; the Raman spectrum is analyzed by the field-point information joint analysis module (12) with the characteristic frequency value f in the basis vector t. i Decompose and use Gaussian function to fit the curve, and then get the water content of each combination type; Step 4: According to the characteristic frequency peak f i and different characteristic frequency peaks f i Gaussian decomposition peak area A i Calculate the field average spectral weighted peak frequency and define the average moisture consolidation degree χ W represents the average bonding strength between water and solid, and substitutes each characteristic peak frequency f i Get the degree of consolidation corresponding to the moisture type.

8. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 7, characterized in that: The method for obtaining the water content of each combination type in this method is specifically as follows: The Raman spectrum is calculated by taking the characteristic frequency value f in the basis vector t i Decompose and use Gaussian function for curve fitting: In the formula, A i are different characteristic frequency peaks f i Gaussian decomposition peak area, the water content of each binding type x i It is expressed as:

9. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 8, characterized in that: The specific method of the consolidation degree corresponding to the moisture type in this method is: Calculate the field average spectral weighted peak frequency F w : Define the average degree of moisture consolidation χ w The average strength of water-solid bonding is as follows: In the formula, F WS represents the characteristic peak frequency of ice. For solid water such as ice, the water binding degree is 1; f0 represents the characteristic peak frequency corresponding to free water when the binding strength between water and solid is the lowest, which is usually the farthest from F in the measured Raman signal. WS Peak frequency f on one side i The extreme value of . Calculate the frequency f of each characteristic peak i Degree of consolidation corresponding to moisture type: For χ i The greater the moisture content, the higher the degree of consolidation.

10. The Raman spectroscopy analysis system for particle water binding strength and content according to claim 7, characterized in that: In the method, a point light source Raman spectrum signal of the degree of binding between water molecules and solid particles is obtained by a point light source optical path (32), and water molecule peak frequency information reflecting the degree of binding between water molecules and solid particles is extracted, and the water molecule and solid binding state information is contained in the peak frequency of the spectrum; a field light source Raman spectrum signal of the degree of binding between water molecules and solid particles is obtained by a field light source optical path (31), and different types of water contents are obtained by inversion from the field Raman spectrum signal.

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