CN112014377B - Method for detecting grade of diamond micropowder by utilizing Raman spectrum and application of method in detecting grade of diamond micropowder - Google Patents

Method for detecting grade of diamond micropowder by utilizing Raman spectrum and application of method in detecting grade of diamond micropowder Download PDF

Info

Publication number
CN112014377B
CN112014377B CN202010973478.8A CN202010973478A CN112014377B CN 112014377 B CN112014377 B CN 112014377B CN 202010973478 A CN202010973478 A CN 202010973478A CN 112014377 B CN112014377 B CN 112014377B
Authority
CN
China
Prior art keywords
raman spectrum
diamond
grade
detecting
peak
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010973478.8A
Other languages
Chinese (zh)
Other versions
CN112014377A (en
Inventor
周建斌
张学涛
周波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhengzhou Jianbin Electronic Technology Co ltd
Original Assignee
Zhengzhou Jianbin Electronic Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhengzhou Jianbin Electronic Technology Co ltd filed Critical Zhengzhou Jianbin Electronic Technology Co ltd
Priority to CN202010973478.8A priority Critical patent/CN112014377B/en
Publication of CN112014377A publication Critical patent/CN112014377A/en
Application granted granted Critical
Publication of CN112014377B publication Critical patent/CN112014377B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • G01N21/64—Fluorescence; Phosphorescence

Landscapes

  • Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

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

Description

Method for detecting grade of diamond micropowder by utilizing Raman spectrum and application of method in detecting grade of diamond micropowder
Technical Field
The invention belongs to the technical field of superhard material detection, and particularly relates to a method for detecting a diamond micro powder grade by utilizing Raman spectrum and application of the method in detecting the diamond micro powder grade.
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 scientific technology, the demand of diamond micro powder in the market is larger and larger, and the demand of quality is also higher and higher. For diamond micropowder, factors influencing quality include particle strength (grade), particle size composition, particle shape, impurity content, etc. There are relatively well-established examination methods for the particle size composition, particle shape, impurity content, etc., of the fine powder, but there is no method for examining the particle strength (grade) of the fine powder. The current method for controlling the grade of the diamond micropowder can only control the grade of the micropowder by controlling the grade of the monocrystalline diamond raw material. Once the single crystal diamond particles were micronized, no method was used to verify their grade. This causes great trouble and uncertainty in quality control of both production units and usage units of the micropowder.
The invention creatively invents a method for analyzing and judging the grade of diamond micro powder by utilizing the characteristics of Raman spectrum analysis. Thereby providing an effective quality inspection and control means for the production and use units of the diamond micro powder.
Disclosure of Invention
The invention provides a method for detecting the grade of diamond micro powder by utilizing Raman spectrum and application of the method in detecting the grade of diamond micro powder. The method can accurately detect the grade of the diamond micro powder, realizes the quality control 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. The Raman spectrum of the diamond micro powder has two obvious Raman characteristic peaks which are respectively expressed as f 1 And f 2 . The raman spectrum of the diamond micropowder is analyzed into two curves, one is a raman spectrum curve and the other is a fluorescence background curve, as shown in fig. 1B. The patent finds that the intensity of the diamond micropowder is directly proportional to an exponential function of the sum of the intensities of two Raman characteristic peaks, inversely proportional to the integral intensity of the fluorescent background, and f 1 The cube root of the peak position shift of the characteristic peak is inversely proportional. And then a mathematical model and a calculation method for analyzing the strength grade of the diamond micro powder by utilizing Raman spectrum are obtained through research. The specific model and algorithm are described below.
The invention is realized by the following technical proposal
A method for detecting diamond micropowder grade by utilizing raman spectrum, comprising the following steps:
s1, detecting a Raman spectrum intensity value and a fluorescence intensity value of a diamond micro powder sample, and f 1 Peak position of raman spectrum peak;
s2, calculating according to the following formula to obtain the diamond grade
Wherein P represents the grade of diamond micropowder and is the average value of q test results; q represents the number of tests and the value range is 1-1000 times; d, d j Represents f 1 Peak position of Raman spectrum is relative to 1333 wave number offset; t (T) j A fluorescence intensity integrated value indicating the jth time; f (f) 1j Represents the peak-to-peak intensity of the j-th diamond raman spectrum 1333; f (f) 2j Represents the peak-to-peak intensity of the j-th diamond raman spectrum 3140; n representsA power exponent; k represents a slope; b represents the intercept.
Further, the detection system for detecting the fluorescence intensity and the raman spectrum intensity of the diamond micro powder 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 positioned 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 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 figure 1.
Further, the fluorescence intensity integrated value is obtained by the formula (2):
wherein T is j Represents the integrated value of fluorescence intensity, t i The fluorescence intensity value of the ith pixel point on the Raman spectrum, i represents the position of the pixel point on the Raman spectrum, 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 ending point, and the values are 1, 2, 3 and 4 … … 2048.
Further, f 1 The peak position wave number shift d of the characteristic peak is calculated as follows:
d j ＝1333-f 1jw (3)
wherein d j F representing the jth time 1 Peak position wave number offset of characteristic peak, f 1jw F representing the j-th sample to be tested 1 Actual peak position wave numbers of the raman characteristic peaks.
Further, n in the formula (1) has a value of 1.0-2.0.
Further, n in the formula (1) has a value of 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 and 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 detection and control of diamond micro powder production and application enterprises. Lays a foundation for stabilizing and improving the quality of the diamond micropowder product.
No method was available prior to the present invention to quantitatively detect the grade of diamond micropowder. The invention provides a high-efficiency detection method for diamond differential grade detection.
Drawings
Figure 1 shows a raman spectrum of a diamond micropowder,
FIG. 2 shows a schematic diagram of a detection system for detecting Raman spectrum intensity of diamond micropowder according to the invention.
Detailed Description
The following detailed description of the present invention is provided to facilitate understanding of the technical solution of the present invention, but is not intended to limit the scope of the present invention.
The invention provides a system for detecting Raman spectrum of a diamond micropowder sample, which 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 platform is arranged right below the probe and is used for containing samples. Each device is connected with a power supply, and measurement can be performed by turning on the power supply.
The invention also provides a method for detecting the Raman spectrum of the diamond micropowder by using the Raman spectrum detection system, which comprises the following steps:
placing a diamond micro powder sample to be detected on a sample table, enabling laser emitted by a laser to irradiate the diamond micro powder sample to be detected through a probe, and exciting the sample to be detected to generate a Raman spectrum and a fluorescence spectrum;
transmitting the detected Raman spectrum information to a spectrometer connected with the probe by the probe;
and converting the Raman spectrum signal into a digital signal by the spectrometer, and transmitting the digital signal to a computer to obtain the Raman spectrum and the fluorescence spectrum of the diamond micropowder sample.
The invention also provides a method for detecting the grade of the diamond micro powder by utilizing the Raman spectrum, which comprises the following steps: s1, detecting a Raman spectrum intensity value and a fluorescence intensity value and f of the diamond micro powder sample according to the method 1 Peak position f of Raman spectrum peak 1w ；
S2, substituting the sample into the following formula (1) to calculate the grade of the diamond sample to be measured,
d j ＝1333-f 1jw (3)
in the formula (1), P represents the grade of diamond micro powder and is the average value of q test results; q represents the number of tests and the value range is 1-1000 times; d, d j Represents f 1 Peak position of Raman spectrum is relative to 1333 wave number offset; t (T) j A fluorescence intensity integrated value indicating the jth time; f (f) 1j Represents the peak-to-peak intensity of the j-th diamond raman spectrum 1333; f (f) 2j Represents the peak-to-peak intensity of the j-th diamond raman spectrum 3140; n represents a power exponent; k represents a slope; b represents the intercept.
In the formula (2), the amino acid sequence of the compound, j represents the integrated value of fluorescence intensity, t i The fluorescence intensity value of the ith pixel point on the Raman spectrum, i represents the position of the pixel point on the Raman spectrum, the values are 1, 2, 3 and 4 … … i, m represents the starting point of integration, the values are 1, 2, 3 and 4 … … 2048, and h represents the integrationEndpoint, take the values 1, 2, 3, 4 … … 2048.
In the formula (3), d j F representing the jth time 1 Peak position wave number offset of characteristic peak, f 1jw F representing the j-th sample to be tested 1 Actual peak position wave numbers of the raman characteristic peaks.
In the formula (1), the gradient k value and the intercept b value are determined to be different values according to specific conditions, wherein the k value can be 0.5-2, and the b value can be 0.01-1.
The invention provides a method for detecting the grade of diamond micro powder by utilizing Raman spectrum and application of the method in the detection of the grade of diamond micro powder. The method can accurately determine the grade of the diamond micro powder and provide guarantee for quality control of the diamond micro powder.
The invention is illustrated by the following specific examples.
Example 1
According to the method provided by the invention, the Raman spectrum information is collected and tested and analyzed.
4 samples of 40/45 diamond abrasive were selected, numbered D1, D2, D3, D4, 200 grams each.
First, 4 samples were respectively subjected to impact toughness (Ti) test, and then strength grades were converted based on the impact toughness test results (one grade per 20 units), and the results are shown in table 1;
the 4 samples were crushed, diamond micropowder with a particle size of M20/30 was separated according to the micropowder production process, and the grade was tested according to the method of the present invention, and the results are shown in table 1.
In this example, the number of tests q=300; power n=1.2; fluorescence integration range, pixel start m=200, end h=2000; slope k=1.022, intercept b=0.176.
Then, the diamond micropowder samples were examined by the method of the present invention, and the results are shown in Table 1.
Table 1 results of the present invention for testing diamond micropowder grade
The raman test data in table 1 fully shows that the grade change of the diamond micro powder measured by raman spectroscopy is basically consistent with the grade change of the raw material, and the grade difference of the diamond micro powder can be completely distinguished by using the raman spectroscopy of the invention.

Claims (5)

1. A method for detecting diamond micropowder grade by utilizing Raman spectrum, which is characterized by comprising the following steps:
s1, detecting a Raman spectrum intensity value and a fluorescence intensity value of a diamond micro powder sample, and f 1 Peak position of raman spectrum peak;
s2, calculating according to the following formula to obtain the diamond grade
Wherein P represents the grade of diamond micropowder and is the average value of q test results; q represents the number of tests and the value range is 1-1000 times; d, d j Represents f 1 Peak position of Raman spectrum is relative to 1333 wave number offset; t (T) j A fluorescence intensity integrated value indicating the jth time; f (f) 1j Represents the peak-to-peak intensity of the j-th diamond raman spectrum 1333; f (f) 2j Represents the peak-to-peak intensity of the j-th diamond raman spectrum 3140; n represents a power exponent; k represents a slope; b represents an intercept; n has a value of 1.0-2.0;
the fluorescence intensity integrated value is obtained by the formula (2):
wherein T is j Represents the integrated value of fluorescence intensity, t i The fluorescence intensity value of the ith pixel point on the Raman spectrum, i represents the position of the pixel point on the Raman spectrum, the values are 1, 2, 3 and 4 … … i, m represents the integral starting point, and the values are 1, 2, 3 and 4 … … 2048, h represents an integration end point, and the values are 1, 2, 3 and 4 … … 2048;
f 1 the peak position wave number shift d of the characteristic peak is calculated as follows:
d j ＝1333-f 1jw (3)
wherein d j F representing the jth time 1 Peak position wave number offset of characteristic peak, f 1jw F representing the j-th sample to be tested 1 Actual peak position wave numbers of the raman characteristic peaks.
2. The method for detecting diamond micro powder grade according to claim 1, wherein the detection system for detecting the fluorescence intensity and 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 disposed directly below the probe.
3. The method of detecting diamond micropowder grade according to claim 2, wherein the method of detecting using the detection system comprises the steps of:
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 Raman spectrum information and transmits the Raman spectrum information to a spectrometer connected with the probe;
and converting the Raman spectrum signal into a digital signal by the spectrometer, and transmitting the digital signal to a computer to obtain the Raman spectrum and the fluorescence spectrum of the diamond sample.
4. The method for detecting diamond micropowder grade according to claim 1, wherein n in the formula (1) has a value of 1.2.
5. Use of the method for detecting diamond micropowder grade according to any one of claims 1 to 4 in diamond micropowder grade detection.
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)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010973478.8A CN112014377B (en) 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

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010973478.8A CN112014377B (en) 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

Publications (2)

Publication Number Publication Date
CN112014377A CN112014377A (en) 2020-12-01
CN112014377B true CN112014377B (en) 2023-08-22

Family

ID=73522609

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010973478.8A Active CN112014377B (en) 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

Country Status (1)

Country Link
CN (1) CN112014377B (en)

Citations (6)

* 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
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

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9581553B2 (en) * 2014-10-18 2017-02-28 Dong-Shyogn Pan Examination method for distinguishing between natural diamond and synthetic CVD/HPHT diamonds

Patent Citations (6)

* 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
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

Also Published As

Publication number Publication date
CN112014377A (en) 2020-12-01

Similar Documents

Publication Publication Date Title
CN102985807B (en) Streaming particle analysing device and streaming particle analysis method
US9581553B2 (en) Examination method for distinguishing between natural diamond and synthetic CVD/HPHT diamonds
CN102954976A (en) Method for quantitatively examining center segregations of wire rod
WO2021196416A1 (en) Optical fiber raman system and method for online detection of tungsten flotation concentrate grades
CN107340276A (en) A kind of method of multiple element content in quick measure rare earth metal/alloy
CN106908436B (en) The analysis ranking method of manganese sulfide type impurity in steel based on calibration curve
CN108593649A (en) A kind of method of qualitative and quantitative test analysis steel inclusion
CN104655607A (en) Detection method of antimony sulfide mineral grade in flotation froth layer
CN104111264A (en) Methods for quickly detecting content of heavy metal elements in rice and evaluating comprehensive pollution index of heavy metal elements
McWhirt et al. Rapid analysis of elemental concentrations in compost via portable X-ray fluorescence spectrometry
CN101799395B (en) Method for preparing and quantifying metallurgical reference substance for grain fineness distribution of inclusions in steel
CN111999260B (en) Method for identifying spodumene-containing pegmatite by thermal infrared spectroscopy and application of thermal infrared spectroscopy
CN111272686B (en) Hyperspectral detection method for iron grade of iron ore concentrate powder
CN106546574A (en) The spectrum analyses and bearing calibration of trace nitrogen in a kind of steel
CN104614283B (en) A kind of analysis method of corresponding object phase change in metal material heat treatment process
CN102279202A (en) Method for measuring chemical compositions in molten iron of blast furnace by X-ray fluorescence spectrometry
CN104297206A (en) Quick liquid milk brand identifying method
CN112014377B (en) Method for detecting grade of diamond micropowder by utilizing Raman spectrum and application of method in detecting grade of diamond micropowder
CN108072747B (en) Quantitative estimation method for inclusion area of high-temperature alloy
CN109668871A (en) The direct-reading spectrometer analysis method of trace amount Ti in a kind of steel
JP5885168B2 (en) Method and apparatus for analyzing soil geological traits
CN105547777A (en) A preparing method of a pig iron standard sample
Davis et al. Developments in automated reflectance microscopy of coal
CN111272617B (en) Method for measuring different mineral particle size distribution characteristics of massive rock sample
Luo et al. An effective solution to simultaneously analyze size, mass and number concentration of polydisperse nanoplastics in a biological matrix: Asymmetrical flow field fractionation coupled with a diode array detector and multiangle light scattering

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant