CN112014377A - Method for detecting grade of diamond micro powder by using Raman spectrum and application of method in detection of grade of diamond micro powder - Google Patents

Method for detecting grade of diamond micro powder by using Raman spectrum and application of method in detection of grade of diamond micro powder Download PDF

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CN112014377A
CN112014377A CN202010973478.8A CN202010973478A CN112014377A CN 112014377 A CN112014377 A CN 112014377A CN 202010973478 A CN202010973478 A CN 202010973478A CN 112014377 A CN112014377 A CN 112014377A
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grade
diamond
raman spectrum
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micro powder
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CN112014377B (en
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周建斌
张学涛
周波
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Zhengzhou Jianbin Electronic Technology Co ltd
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract

The invention provides a method for detecting the grade of diamond micro powder by using Raman spectrum and application thereof in the grade detection of the diamond micro powder. The method comprises the steps of detecting the fluorescence intensity value and the Raman spectrum intensity value of a diamond micro powder sample; then according to the formula

Description

Method for detecting grade of diamond micro powder by using Raman spectrum and application of method in detection of grade of diamond micro powder
Technical Field
The invention belongs to the technical field of detection of superhard materials, and particularly relates to a method for detecting the grade of diamond micro powder by using Raman spectrum and application of the method in detecting the grade of diamond micro powder.
Background
The diamond micro powder has high hardness and good wear resistance, and is widely used for cutting, grinding, drilling, polishing and the like. With the development and progress of science and technology, the demand of the market for diamond micro powder is larger and larger, and the requirement on quality is higher and higher. For the diamond micropowder, factors affecting the quality include particle strength (grade), particle size composition, particle shape, impurity content and the like. There are relatively mature methods for examining items such as the particle size composition, particle shape, and impurity content of the fine powder, but there is no method for examining the particle strength (grade) of the fine powder. The existing method for controlling the grade of the diamond micro-powder can only control the grade of the micro-powder by controlling the grade of the raw material of the single crystal diamond. Once the single crystal diamond particles are micronized, there is no way to examine their grade. This brings about a great trouble and uncertainty in quality control of both production units and use units of the fine powder.
Aiming at the problem, the invention creatively invents a method for analyzing and judging the grade of the diamond micro powder by utilizing the characteristic of Raman spectrum analysis. Thereby providing an effective quality inspection and control means for the production and use units of the diamond micropowder.
Disclosure of Invention
Aiming at the problems, the invention provides a method for detecting the grade of diamond micro powder by using Raman spectrum and application thereof in detecting the grade of diamond micro powder. The method can accurately detect the grade of the diamond micro powder, realizes the control of the quality of the diamond micro powder, is convenient and quick, and has good application effect. The Raman spectrum of the diamond micropowder is shown in figure 1A. Two obvious Raman characteristic peaks are shown on the Raman spectrum of the diamond micropowder respectively as f1And f2. The raman spectrum of the diamond micropowder is analyzed into two curves, as shown in fig. 1B, one is a raman spectrum curve, and the other is a fluorescence background curve. The patent finds that the intensity of the diamond micro powder is in direct proportion to an exponential function of the sum of the intensities of two Raman characteristic peaks, in inverse proportion to the integral intensity of a fluorescence background, and in f1The cube root of the peak position offset of a characteristic peak is inversely proportional. Then, a mathematical model and a calculation method for analyzing the strength grade of the diamond micro powder by using the Raman spectrum are obtained through exploration. Specific models and algorithms are described below.
The invention is realized by the following technical scheme
A method for detecting the grade of diamond micro powder by using Raman spectrum comprises the following steps:
s1, detecting the Raman spectrum intensity value and the fluorescence intensity value of the diamond micro powder sample and f1Peak position of raman spectrum peak;
s2, calculating the diamond grade according to the following formula
Figure BDA0002684928590000021
In the formula, P represents the grade of the diamond micro powder and is the average value of the test results of q times; q represents the test times, and the value range is 1-1000 times; djDenotes f1The relative 1333 wave number offset of the peak position of the Raman spectrum; t isjRepresents the fluorescence intensity integrated value of the j-th time; f. of1jRepresents the peak intensity of the j-th diamond Raman spectrum 1333; f. of2jThe peak intensity of a diamond Raman spectrum 3140 peak at the jth time is represented; n represents a power exponent; k represents a slope; b denotes the intercept.
Further, the detection system for detecting the fluorescence intensity and the raman spectrum intensity of the diamond micro powder sample in step S1 is specifically as follows: the system comprises a sample stage, a laser, a probe, a spectrometer and a computer; the probe is electrically connected with the laser, the probe is also electrically connected with the spectrometer, and the spectrometer is electrically connected with the computer; the sample stage is arranged directly below the probe, as shown in fig. 2.
Further, the method for detecting by adopting the detection system comprises the following steps: laser emitted by the laser irradiates the diamond micro powder sample to be detected through the probe, and excites the sample to be detected to generate a Raman spectrum and a fluorescence spectrum; the probe detects the Raman spectrum information and transmits the Raman spectrum information to a spectrometer connected with the probe; the spectrometer converts the raman spectrum signal into a digital signal and transmits the digital signal to a computer, so that the raman spectrum and the fluorescence spectrum of the diamond sample are obtained, as shown in fig. 1.
Further, the fluorescence intensity integrated value is obtained by formula (2):
Figure BDA0002684928590000022
in the formula, TjRepresents the integrated value of fluorescence intensity, tiThe fluorescence intensity value of the ith pixel point on the Raman spectrogram is represented, i represents the point position of the pixel on the Raman spectrogram, the values are 1, 2, 3 and 4 … … i, m represents the integration starting point, the values are 1, 2, 3 and 4 … … 2048, h represents the integration end point, and the values are 1, 2, 3 and 4 … … 2048.
Further, f1The peak position wave number offset d of the characteristic peak is calculated as follows:
dj＝1333-f1jw (3)
in the formula (d)jF for j times1Peak position wave number offset of characteristic peak, f1jwF representing the j-th sample to be measured1Actual peak wavenumber of the raman characteristic peak.
Further, the value of n in the formula (1) is 1.0-2.0.
Further, the value of n in the formula (1) is 1.2.
The method for detecting the grade of the diamond micro powder is applied to the grade detection of the diamond micro powder.
Compared with the prior art, the invention has the following positive beneficial effects
The method for detecting the grade of the diamond micro powder through the Raman spectrum can effectively determine the grade of the diamond micro powder, and provides a scientific and effective detection method for quality inspection and control of diamond micro powder production and application enterprises. Lays a foundation for the stability and improvement of the quality of the diamond micro powder product.
Prior to the present invention, there was no method to quantitatively detect the grade of diamond micropowder. The invention provides an efficient detection method for diamond differential grade detection.
Drawings
Figure 1 shows a raman spectrum of a diamond micropowder,
FIG. 2 is a schematic diagram of a detection system for detecting Raman spectrum intensity of diamond micropowder according to the present invention.
Detailed Description
The present invention will be described in more detail with reference to the following embodiments for understanding the technical solutions of the present invention, but the present invention is not limited to the scope of the present invention.
The invention provides a system for detecting Raman spectrum of a diamond micro powder sample, which comprises a sample table, a laser, a probe, a spectrometer and a computer, wherein the sample table is used for storing diamond micro powder; the probe is electrically connected with the laser, the probe is also electrically connected with the spectrometer, and the spectrometer is electrically connected with the computer; the sample stage is arranged under the probe and used for containing a sample. Each device is connected with a power supply, and the power supply is turned on to carry out measurement.
The invention also provides a method for detecting the Raman spectrum of the diamond micro powder by using the detection system of the Raman spectrum, which comprises the following steps:
placing a diamond micro powder sample to be detected on a sample table, and irradiating laser emitted by a laser on the diamond micro powder sample to be detected through a probe to excite the diamond micro powder sample to be detected to generate a Raman spectrum and a fluorescence spectrum;
the probe transmits the detected Raman spectrum information to a spectrometer connected with the probe;
the spectrometer converts the Raman spectrum signal into a digital signal and transmits the digital signal to the computer, and the Raman spectrum and the fluorescence spectrum of the diamond micro powder sample are obtained.
The invention also provides a method for detecting the grade of the diamond micro powder by using the Raman spectrum, which comprises the following steps: s1, detecting the Raman spectrum intensity value, the fluorescence intensity value and the f of the diamond micro powder sample according to the method1Peak position f of Raman spectrum peak1w；
S2, substituting the obtained product into the following formula (1), calculating the grade of the diamond sample to be measured,
Figure BDA0002684928590000031
Figure BDA0002684928590000032
dj＝1333-f1jw (3)
in the formula (1), P represents the grade of the diamond micro powder and is the average value of the test results of q times; q represents the test times, and the value range is 1-1000 times; djDenotes f1The relative 1333 wave number offset of the peak position of the Raman spectrum; t isjRepresents the fluorescence intensity integrated value of the j-th time; f. of1jRepresents the peak intensity of the j-th diamond Raman spectrum 1333; f. of2jThe peak intensity of a diamond Raman spectrum 3140 peak at the jth time is represented; n represents a power exponent; k represents a slope; b denotes the intercept.
In the formula (2), the reaction mixture is,jrepresents the integrated value of fluorescence intensity, tiThe fluorescence intensity value of the ith pixel point on the Raman spectrogram is represented, i represents the point position of the pixel on the Raman spectrogram, the values are 1, 2, 3 and 4 … … i, m represents the integration starting point, the values are 1, 2, 3 and 4 … … 2048, h represents the integration end point, and the values are 1, 2, 3 and 4 … … 2048.
In the formula (3), djF for j times1Peak position wave number offset of characteristic peak, f1jwF representing the j-th sample to be measured1Actual peak wavenumber of the raman characteristic peak.
In the formula (1), different values of the slope k value and the intercept b value are determined according to specific conditions, wherein the value of k can be 0.5-2, and the value of b can be 0.01-1.
The invention provides a method for detecting the grade of diamond micro powder by using Raman spectrum and application in the grade detection of the diamond micro powder. The method can accurately determine the grade of the diamond micro powder and provides guarantee for the quality control of the diamond micro powder.
The present invention is illustrated by the following specific examples.
Example 1
According to the method provided by the invention, the Raman spectrum information is collected for test analysis.
40/45 diamond abrasive samples were selected, numbered D1, D2, D3, D4, 200 grams each.
Firstly, respectively testing 4 samples by using impact toughness (Ti), and then converting the impact toughness test results into strength grades (one grade per 20 units), wherein the results are shown in a table 1;
the 4 samples were then crushed and sorted according to the micropowder production process to give diamond micropowder of size specification M20/30, and then tested for grade according to the method of the invention, with the results shown in table 1.
In this example, the number of tests q is 300; the power index n is 1.2; the fluorescence integration range is that the pixel starting point m is 200 and the end point h is 2000; slope k is 1.022 and intercept b is 0.176.
Then, the diamond micro powder sample is detected by the method of the invention, and the result is shown in table 1.
Table 1 grade results of diamond micro powder measured by the present invention
Figure BDA0002684928590000051
The raman test data in table 1 fully indicates that the change of the grade of the diamond fine powder measured by the raman spectroscopy is basically consistent with the grade change of the raw material, and the difference of the grade of the diamond fine powder can be completely distinguished by the raman spectroscopy.

Claims (8)

1. A method for detecting the grade of diamond micro powder by using Raman spectrum is characterized by comprising the following steps:
s1, detecting the Raman spectrum intensity value and the fluorescence intensity value of the diamond micro powder sample and f1Peak position of raman spectrum peak;
s2, calculating the diamond grade according to the following formula
Figure FDA0002684928580000011
In the formula, P represents the grade of the diamond micro powder and is the average value of the test results of q times; q represents the test times, and the value range is 1-1000 times; djDenotes f1The relative 1333 wave number offset of the peak position of the Raman spectrum; t isjRepresents the fluorescence intensity integrated value of the j-th time; f. of1jRepresents the peak intensity of the j-th diamond Raman spectrum 1333; f. of2jThe peak intensity of a diamond Raman spectrum 3140 peak at the jth time is represented; n represents a power exponent; k represents a slope; b denotes the intercept.
2. The method for detecting the grade of the diamond micropowder according to claim 1, wherein the detection system for detecting the fluorescence intensity and the Raman spectrum intensity of the diamond micropowder sample in the step S1 is specifically as follows:
the system comprises a sample stage, a laser, a probe, a spectrometer and a computer; the probe is electrically connected with the laser, the probe is also electrically connected with the spectrometer, and the spectrometer is electrically connected with the computer; the sample stage is arranged right below the probe.
3. The method for detecting the grade of the diamond micropowder according to claim 2, wherein the method for detecting by using the detection system comprises the following steps:
laser emitted by the laser irradiates the diamond micro powder sample to be detected through the probe, and excites the sample to be detected to generate a Raman spectrum and a fluorescence spectrum;
the probe detects the Raman spectrum information and transmits the Raman spectrum information to a spectrometer connected with the probe;
the spectrometer converts the Raman spectrum signal into a digital signal and transmits the digital signal to the computer, and the Raman spectrum and the fluorescence spectrum of the diamond sample are obtained.
4. The method for detecting the grade of fine diamond powder according to claim 1, wherein the fluorescence intensity integral value is obtained by the formula (2):
Figure FDA0002684928580000012
in the formula, TjRepresents the integrated value of fluorescence intensity, tiI table representing the fluorescence intensity value of the ith pixel point on the Raman spectrogramThe point positions of pixels on the Raman spectrogram are shown as 1, 2, 3 and 4 … … i, m represents an integration starting point, 1, 2, 3 and 4 … … 2048, h represents an integration end point and is 1, 2, 3 and 4 … … 2048.
5. The method for detecting the grade of fine diamond powder according to claim 1, wherein f is1The peak position wave number offset d of the characteristic peak is calculated as follows:
dj＝1333-f1jw (3)
in the formula (d)jF for j times1Peak position wave number offset of characteristic peak, f1jwF representing the j-th sample to be measured1Actual peak wavenumber of the raman characteristic peak.
6. The method for detecting the grade of the diamond micropowder according to claim 1, wherein the value of n in the formula (1) is 1.0-2.0.
7. The method for detecting the grade of the diamond micropowder according to claim 5, wherein n in the formula (1) takes a value of 1.2.
8. Use of the method for testing the grade of diamond micropowder according to any one of claims 1 to 7 for testing the grade of diamond micropowder.
CN202010973478.8A 2020-09-16 2020-09-16 Method for detecting grade of diamond micropowder by utilizing Raman spectrum and application of method in detecting grade of diamond micropowder Active CN112014377B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1585895A (en) * 2001-09-12 2005-02-23 杰桑企业 Examining a diamond
CN103364387A (en) * 2012-04-01 2013-10-23 深圳市宇驰检测技术有限公司 Laser Raman detection method of malachite green
US20160109374A1 (en) * 2014-10-18 2016-04-21 Dong-Shyogn Pan Examination method for distinguishing between natural diamond and synthetic cvd/hpht diamonds
EP3225976A1 (en) * 2016-03-29 2017-10-04 Dong-Shyogn Pan Method of rapid identification of natural and synthetic diamonds using third-order raman spectra
CN107305185A (en) * 2016-04-25 2017-10-31 潘栋雄 Using Raman method naturally with synthesizing diamond is distinguished in the characteristic peak of three rank spectrum
CN107305188A (en) * 2016-04-25 2017-10-31 潘栋雄 The detection method of diamond color grade
CN208399381U (en) * 2018-06-19 2019-01-18 捷斯奥企业有限公司 Diamond dust intensity measuring equipment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1585895A (en) * 2001-09-12 2005-02-23 杰桑企业 Examining a diamond
CN103364387A (en) * 2012-04-01 2013-10-23 深圳市宇驰检测技术有限公司 Laser Raman detection method of malachite green
US20160109374A1 (en) * 2014-10-18 2016-04-21 Dong-Shyogn Pan Examination method for distinguishing between natural diamond and synthetic cvd/hpht diamonds
EP3225976A1 (en) * 2016-03-29 2017-10-04 Dong-Shyogn Pan Method of rapid identification of natural and synthetic diamonds using third-order raman spectra
CN107305185A (en) * 2016-04-25 2017-10-31 潘栋雄 Using Raman method naturally with synthesizing diamond is distinguished in the characteristic peak of three rank spectrum
CN107305188A (en) * 2016-04-25 2017-10-31 潘栋雄 The detection method of diamond color grade
CN208399381U (en) * 2018-06-19 2019-01-18 捷斯奥企业有限公司 Diamond dust intensity measuring equipment

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