CN114486899A - Method for identifying natural irradiation diamond and laboratory artificial irradiation treatment diamond - Google Patents
Method for identifying natural irradiation diamond and laboratory artificial irradiation treatment diamond Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 107
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000012360 testing method Methods 0.000 claims abstract description 62
- 230000003287 optical effect Effects 0.000 claims abstract description 30
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- 230000001788 irregular Effects 0.000 claims abstract description 4
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- 238000004458 analytical method Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000010437 gem Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
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- 238000007654 immersion Methods 0.000 description 3
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- ZZIZZTHXZRDOFM-XFULWGLBSA-N tamsulosin hydrochloride Chemical compound [H+].[Cl-].CCOC1=CC=CC=C1OCCN[C@H](C)CC1=CC=C(OC)C(S(N)(=O)=O)=C1 ZZIZZTHXZRDOFM-XFULWGLBSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000000701 chemical imaging Methods 0.000 description 1
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- 238000012850 discrimination method Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
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- 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
- G01N21/84—Systems specially adapted for particular applications
- G01N21/87—Investigating jewels
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/06—Illumination; Optics
- G01N2201/061—Sources
- G01N2201/06113—Coherent sources; lasers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/10—Scanning
- G01N2201/102—Video camera
Abstract
The invention discloses a method for identifying natural irradiation diamonds and laboratory artificial irradiation treatment diamonds, which comprises the following steps: building a test optical platform, preparing a sample and testing the sample; drawing a surface scanning spectrum pattern or a volume scanning spectrum pattern; judging the spectrum pattern, if the 2D spectrum pattern shows smaller irradiation spots with obvious multi-point gradual change, judging the diamond to be naturally irradiated, and if the 2D spectrum pattern shows larger irradiation spots with uniform spots and integral directivity, judging the diamond to be artificially irradiated in a laboratory; if the 3D spectral graph shows irregular strip-shaped gradual change in the depth direction, the diamond is judged to be naturally irradiated; if the irradiation spots obviously uniformly and gradually changed on one side in the depth direction are displayed, the diamond is judged to be artificially irradiated in the laboratory. The invention can effectively distinguish natural irradiation diamonds from laboratory artificial irradiation and provides scientific reference basis for the identification of color cause of the irradiation diamonds.
Description
[ technical field ]
The invention relates to gem identification, in particular to an identification method of natural irradiation diamonds and laboratory artificial irradiation treatment diamonds.
[ background art ]
In the market, a laboratory artificial irradiation source such as an electron beam is often adopted to irradiate the diamond with unattractive color, so that the diamond is colorless and bright blue, green, pink and other colors. The price of the irradiation treated diamond is greatly different from that of the natural diamond without irradiation treatment, so that the identification of the color cause of the diamond has important guiding significance for the commercial trade and government regulation of the diamond. However, the identification of the diamond color cause is a difficult problem for the identification of the diamond, and laboratories mainly rely on manual visual inspection and spectral qualitative analysis, and because of the similarity of the two causes, a large number of samples still exist at present and cannot be identified, which affects the development of the diamond market.
Because the artificial irradiation in the laboratory is close to the natural irradiation diamond in principle, irradiation spots are generated on the surface of the diamond and internal crystal lattice vacancies are caused, so that the separation of the artificial irradiation and the natural irradiation by pure spectral line measurement becomes difficult. Meanwhile, the information amount remained on the surface of the diamond is greatly reduced through the later cutting and polishing processing. Typically, the irradiated spot of the finished diamond is not visible to the naked eye and under a conventional microscope. The method brings great challenges to the identification of color cause of laboratory artificial natural irradiation and laboratory artificial irradiation diamonds. At present, the following three methods are mainly used for identification:
1. oil immersion observation method
The color concentrated distribution phenomenon of the color bands of the early laboratory artificial irradiation treated diamonds is different from that of the natural diamonds, and the umbrella shape/color concentrated distribution characteristic of the pavilion/base tip color bands of the laboratory artificial irradiation treated diamonds can be observed by immersing the diamonds in transparent oil such as baby oil as shown in figure 1, so that the laboratory artificial irradiation and the natural irradiation diamonds can be distinguished. However, with the improvement of the laboratory artificial irradiation technology, most of the laboratory artificial irradiation diamonds appearing in the market after 2016 have no umbrella shape/color concentration distribution characteristics, and cannot be identified by adopting an oil immersion observation method.
2. Characteristic of gem of paradoxical theory
The change in internal color centers of diamonds after irradiation is currently confirmed by irradiation experiments (Khomich et al, 2019). The gem detection laboratory qualitatively analyzes whether color centers such as H3, GR1 and NV exist or not and relative intensity thereof and the like mainly through the characteristics of infrared spectrums, ultraviolet spectrums and fluorescence spectrums, further preliminarily judges the color cause of the gem, and if the color presented by the diamond does not accord with the color corresponding to the characteristic color center, the possibility that the color cause belongs to the laboratory manual irradiation is high (Song et al, 2016; Huang et al, 2018, Sinkiang Phoeby, 2019). However, many type IIa diamonds are not or only very pale in color and cannot be identified by the methods described above.
3. Fluorescence imaging method
If the above 1, 2 method is still unable to judge, then the fluorescence luminescence image feature can be observed under Diamond View/DDO, as shown in FIG. 2, a particle of blue in FIG. 2The colored synthetic diamond shows bright orange color (Eaton-
2020), but there are also such phenomena that are not evident in diamonds (Huang et al, 2018), and therefore this method can only be used as a laboratory/natural irradiation diamond color cause-assisted judgment means without judgment evidence.
Therefore, the existing method for distinguishing the artificial/natural irradiation diamonds in the laboratory, the oil immersion observation method and the fluorescence luminescence image method depend on the observation experience, and with the improvement of the irradiation technology, most diamonds irradiated in the market at present cannot observe the phenomenon of color lump concentration; the gemology characteristics are scientific and are the most common qualitative identification method at present, but quantification is difficult, and the irradiation characteristics cannot be intuitively displayed.
[ summary of the invention ]
The invention aims to provide an identification method capable of effectively distinguishing natural irradiation diamonds from laboratory artificial irradiation treatment diamonds.
In order to solve the technical problems, the invention adopts the technical scheme that the method for identifying the natural diamond and the artificial processing diamond comprises the following steps:
101) building a test optical platform, adjusting a light path and setting test parameters;
102) preparing a sample;
103) test samples: testing a sample by using the built testing optical platform, and recording the spectral peak height of a characteristic color center (GR1) of each testing point;
104) drawing a surface scanning spectrum pattern or a volume scanning spectrum pattern;
105) judging the surface scanning spectrum pattern or the volume scanning spectrum pattern, if smaller irradiation spots with obvious multi-point gradual change appear in the 2D spectrum pattern formed by surface scanning, judging the diamond as natural irradiation diamond, and if larger irradiation spots with uniform spots appear, judging the diamond as laboratory artificial irradiation diamond; if the 3D spectrum graph formed by volume scanning shows an irregular strip-shaped gradual change phenomenon in the depth direction, the diamond is judged to be naturally irradiated; or if the phenomenon that one side in the depth direction shows obvious uniform gradual change or the phenomenon that the depth direction shows obvious layering phenomenon, the diamond is judged to be artificially irradiated in the laboratory.
In the above identification method, the test optical platform in step 101 includes a laser, a beam expander, a reflector, a filter, a lens, a slit, a grating prism assembly, an EMCCD detector, a microscope, and an automated moving platform; laser emitted by the laser reaches the beam expander, the beam is expanded by the beam expander, and the expanded laser is transmitted to the optical filter through the first reflector; the laser from the optical filter is transmitted to the microscope by a plurality of second reflectors and then transmitted to the sample by the optical path of the microscope; the single-point and surface/body scanning test of the sample is realized through the automatic mobile platform, after laser irradiates the sample, single-point and surface/body scanning signal data returns to the optical filter along a microscope optical path, then the single-point and surface/body scanning signal data is transmitted to the EMCCD detector through the lens and the slit, and the single-point and surface/body scanning signal data is collected by the EMCCD detector and transmitted to the computer end for analysis.
In the above identification method, the adjusting of the light path includes making the focal point observed in the microscope coincide with the focal point of the laser light path, the setting of the test parameter includes setting the energy of the laser, and the setting of the wavelength range is controlled by the integration of the laser, the optical filter, the lens, the slit, the grating and the prism assembly.
In the above-described discrimination method, the laser was set to an energy of 25mW to 35mW, and the test range was set to 600nm to 800 nm.
In the above identification method, the sample preparation in step 102 includes cutting, grinding, polishing, and placing in a refrigeration temperature control stage; the temperature in the refrigeration temperature control objective table is stabilized below-150 ℃; the refrigeration temperature control objective table is placed on the automatic moving platform, and diamond samples in the refrigeration temperature control objective table are located under the microscope.
In the identification method, in step 103, a color center embodying irradiation characteristics is found out from a scanning matrix, the spectral peak height value of the characteristic color center of each test point of the sample is recorded, the test area is rectangular, and the test area frames the sample; setting scanning step length, and carrying out dot matrix test on the surface scanning according to a bow-shaped test route; for volume scanning, besides the operation according to surface scanning, the scanning depth is also adjusted, and the test is carried out according to the operation of surface scanning layer by layer.
In the above identification method, in step 104, the spectral peak height value in the sample test area is normalized, and the gray scale is used to represent the peak height degree, wherein the dark gray represents the peak height, and the light gray represents the peak height; carrying out normalization processing on the data of the surface scanning to obtain a 2D spectrum graph; and carrying out normalization processing on the volume scanning data, traversing the depth direction one by one to obtain multilayer 2D graphs, and superposing the multilayer 2D spectrum graphs through software to form a 3D spectrum graph.
The invention can effectively judge the color cause of the diamond, effectively distinguish natural irradiation from laboratory artificial irradiation of the diamond, and provide a scientific reference basis for identifying the color cause of the diamond.
[ description of the drawings ]
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a graph of the slight enrichment of the color of the base tip of a prior art laboratory manually irradiated diamond (picture source Paul Johnson et al, 2016).
FIG. 2 is a characteristic diagram of a fluorescence image of a synthetic diamond subjected to irradiation treatment in the prior art (Eaton-
，2020)。
FIG. 3 is a 2D image of a diamond irradiation spot according to an embodiment of the present invention (where a is an image of a natural irradiation spot in a diamond, and b and c are images of a laboratory artificial irradiation spot in a diamond).
FIG. 4 is a 3D image of irradiation spots of a diamond according to an embodiment of the present invention (where a is an image of a natural irradiation spot in a diamond and b and c are images of a laboratory artificial irradiation spot in a diamond).
FIG. 5 is a schematic diagram of sample testing according to an embodiment of the present invention (where a is a single point spectral line test in which only one point in the sample is tested, b is a 2D scan test in which one face in the sample is lattice tested, and c is a 3D scan test in which multiple faces in the sample are lattice tested).
FIG. 6 is a plot of the position of the peak and intensity of the GR1 color center sample according to an embodiment of the invention.
FIG. 7 is a diagram of a test optical bench architecture according to an embodiment of the present invention.
[ detailed description of the invention ]
The identification method of the natural diamond and the artificial diamond forms a dot matrix through spectra and draws images to distinguish the laboratory artificial irradiation diamond and the natural irradiation diamond, and the identification method comprises the following testing steps:
1. building a test environment, adopting a Thermo Fisher 532nm laser and a Thermo Fisher expansion grating, and configuring an EMCCD detector and an Olympus optical microscope system: the system comprises a lens 10X and a numerical aperture 0.25, wherein an optical platform is built, a light path is adjusted, and a scanning test on a sample is realized through an automatic moving platform;
the structure of the test optical platform is shown in fig. 7, and the test optical platform comprises a laser 1, a beam expander 2, a reflector 3, a filter 4, a lens 5, a slit 6, a grating prism assembly 7, an EMCCD detector 8, a microscope 9 and an automatic moving platform 10; pure laser is emitted by a laser 1(532nm) in the graph 7 to reach a beam expander, beam expansion is carried out by the beam expander 2, the laser is transmitted to an optical filter 4 through a reflector 3, the laser is transmitted to a microscope through 3 other reflectors, the laser is transmitted to a sample 11 through a microscope optical path, single-point and surface/body scanning test of the sample is realized through an automatic moving platform 10, single-point and surface/body scanning signal data are transmitted to the optical filter 4, a lens 5 and a slit 6 along the microscope after the laser irradiates the sample, a specific optical signal is transmitted to an EMCCD detector 8 through a grating and prism assembly 7, and the data are collected by the EMCCD detector 8 and transmitted to a computer end for analysis.
2. Preparing a sample, cutting, grinding and polishing a diamond sample, and placing the diamond sample in a Linkman objective table; linkman is refrigeration temperature control equipment, and the temperature can be controlled to be-197 ℃ to 200 ℃ under a water-free cold circulation system; the GR1 zero phonon line can be more obvious by controlling the temperature below-150 ℃. The refrigeration temperature control objective table is placed on an automatic moving platform, and a diamond sample 11 in the refrigeration temperature control objective table is positioned under a microscope.
3. Setting test parameters, setting the energy of a laser to be 30mW, and setting the test range to be 600nm-800nm due to the position of a test peak (GR 1); and adjusting the light path to enable the focus observed in the microscope to coincide with the position of the focusing point of the laser light path.
4. Testing a sample, wherein a testing area is square/rectangular, the size of the testing area is framed according to an actual sample, a scanning step length is set according to the testing requirement of the actual sample, and for 2D surface scanning (in the X-Y direction), a dot matrix test is carried out according to a bow-shaped testing route until the testing is finished; for 3D volume scanning (X-Y-Z direction), in addition to operating in the X-Y direction in 2D surface scanning, the scan depth needs to be set (i.e., Z direction setting, without exceeding the optical limit of depth), and then the test is performed layer by layer according to the operation of surface scanning, as shown in FIG. 5.
5. Finding out the color center GR1 which embodies the irradiation characteristics, and recording the characteristic color center spectrum peak height of each test point of the test sample, as shown in FIG. 6.
6. Drawing a surface scanning spectrum graph, performing normalization processing on peak height values in a sample testing area, respectively representing the degree of the peak height by adopting dark gray and light gray, wherein dark gray spots represent the peak height, light gray represents the peak value, 2D graphs are drawn by adopting OMNIC 2xi software of the Sammerfo company, the OMNIC 2xi software can draw 2D graphs through the changes of the peak height, the peak area and the peak ratio, and the drawn 2D graphs are shown in figure 3. In FIG. 3, a is the image of the naturally irradiated spot in diamond, and b and c are the images of the laboratory artificially irradiated spots in diamond.
7. Drawing a volume scanning spectrum graph, carrying out normalization processing on peak height values in a sample testing area, respectively representing the degree of the peak height by adopting dark gray and light gray, wherein the dark gray represents the peak height, the light gray represents the peak low, and traversing the depth direction (Z direction) one by one; the method comprises the steps of synthesizing by using ImageJ (the software can obtain a 3D graph through 2D graph superposition), or drawing the 3D graph by Matlab (the software can draw the 3D graph through the strength of different layer data point positions and the like), namely superposing the graphs in the Z direction to form the 3D graph, as shown in FIG. 4. In fig. 4, a is the image of the naturally irradiated spot in diamond, and b and c are the images of the laboratory artificially irradiated spots in diamond.
8. And (4) identifying the laboratory artificial irradiation diamond and the natural irradiation diamond according to the 2D graph obtained in the step (6) and/or the 3D graph obtained in the step (7). In the 2D graph, the irradiation spots which show relatively small and obvious multipoint gradual change are natural irradiation diamonds, and the irradiation spots which show large and uniform spots are laboratory artificial irradiation diamonds. Generally, the spot size is less than 1/4 of the sample table area, and the spot is judged to be relatively small; the spot size is determined to be relatively large when the area occupied by the spot size is greater than 1/2 of the area of the sample table. In the 3D graph, if irradiation spots with irregular strip-shaped gradual changes appear in the depth direction, the diamond is judged to be a natural irradiation diamond; or if the irradiation spot with obvious uniform gradual change appears on one side in the depth direction, or the irradiation spot with obvious layering phenomenon appears in the depth direction, the diamond is judged to be artificially irradiated in the laboratory. .
For naturally irradiated diamonds, the irradiation around their environment is relatively random and usually exhibits a point-like non-uniform distribution. The irradiation source of the laboratory manual irradiation is relatively fixed, and the irradiation spots are relatively large and uniform. This method was not investigated for post-irradiation heat-treated diamonds, and was not applicable to diamonds with insignificant peak positions for GR 1.
The embodiment of the invention utilizes a spectral imaging technology to measure the color center (GR1) related to irradiation in the diamond, forms a dot matrix in 2D and 3D spaces, and draws a dot matrix image through characteristic analysis of the dot matrix, so that the color cause of the diamond can be effectively judged, the artificial irradiation in a laboratory and the natural irradiation diamond can be effectively distinguished, scientific reference basis is provided for identifying the color cause of the diamond, and the method has important practical significance for exciting the market vitality of the colored diamond and improving the circulation supervision capability of the colored diamond.
The above nouns explain:
laboratory artificial irradiation of diamonds: the method is characterized in that the original color of the diamond is changed by irradiating the surface of the diamond with high-energy rays such as electron beams in a laboratory environment.
Natural irradiation of diamond: in nature, the color of diamonds is changed by radioactive minerals or the environment.
GR1 color center: the diamond sample is characterized by the characteristic peak position at 740-742nm of the absorption/emission spectrum.
Claims (7)
1. A method for identifying natural irradiation diamonds and laboratory artificial irradiation treatment diamonds is characterized by comprising the following steps:
101) building a test optical platform, adjusting a light path and setting test parameters;
102) preparing a sample;
103) test samples: testing a sample by using the built testing optical platform, and recording the characteristic color center (GR1) spectral peak height of each testing point;
104) drawing a surface scanning spectrum pattern or a volume scanning spectrum pattern;
105) judging the surface scanning spectrum pattern or the volume scanning spectrum pattern, if smaller irradiation spots with obvious multi-point gradual change appear in the 2D spectrum pattern formed by surface scanning, judging the diamond as natural irradiation diamond, and if larger irradiation spots with uniform spots appear, judging the diamond as laboratory artificial irradiation diamond; if the 3D spectrum graph formed by volume scanning shows an irregular strip-shaped gradual change phenomenon in the depth direction, the diamond is judged to be naturally irradiated; or if one side in the depth direction shows obvious uniform gradual change phenomenon, or the depth direction shows obvious layering phenomenon, the diamond is judged to be artificially irradiated in the laboratory.
2. The method of claim 1, wherein the test optical stage in step 101 comprises a laser, a beam expander, a mirror, a filter, a lens, a slit, a grating prism assembly, an EMCCD detector, a microscope, and an automated motion stage; laser emitted by the laser reaches the beam expander, the beam is expanded by the beam expander, and the expanded laser is transmitted to the optical filter through the first reflector; the laser light coming out of the optical filter is transmitted to the microscope by a plurality of second reflectors and then transmitted to the sample through the optical path of the microscope; the single-point and surface/body scanning test of the sample is realized through the automatic mobile platform, after laser irradiates the sample, single-point and surface/body scanning signal data return to the optical filter along a microscope optical path, then the single-point and surface/body scanning signal data pass through the lens and the slit, the grating prism assembly is transmitted to the EMCCD detector, and the single-point and surface/body scanning signal data are collected by the EMCCD detector and transmitted to the computer end for analysis.
3. The authentication method of claim 2, wherein adjusting the optical path comprises coinciding a focal point observed in the microscope with a focal point position of the laser optical path, and wherein setting the test parameter comprises setting an energy of the laser to set a wavelength range by an integral control of the laser, the filter, the lens, the slit, the grating, and the prism assembly.
4. An authentication method according to claim 3, wherein the laser is set at an energy of 25mW to 35mW, and the test range is set at 600nm to 800 nm.
5. The method of claim 1, wherein the preparing the sample in step 102 comprises cutting, grinding, polishing the sample, placing in a refrigerated temperature controlled stage; the temperature in the refrigeration temperature control objective table is stabilized below-150 ℃; the refrigeration temperature control objective table is placed on the automatic moving platform, and diamond samples in the refrigeration temperature control objective table are located under the microscope.
6. The identification method according to claim 1, wherein in step 103, a color center representing the irradiation characteristic is found in the scanning matrix, the spectral peak height value of the characteristic color center of each test point of the sample is recorded, the test area is rectangular, and the test area frames the sample; setting scanning step length, and carrying out dot matrix test on the surface scanning according to a bow-shaped test route; for volume scanning, besides the operation according to surface scanning, the scanning depth is also adjusted, and the test is carried out according to the operation of surface scanning layer by layer scanning.
7. The method according to claim 6, wherein in step 104, the peak height of the spectrum in the test area of the sample is normalized by using gray scale to represent the degree of the peak height, wherein dark gray represents high peak value and light gray represents low peak value; carrying out normalization processing on the surface scanning data to obtain a 2D spectrum graph; and carrying out normalization processing on the volume scanning data, traversing the depth direction one by one to obtain multilayer 2D graphs, and superposing the multilayer 2D spectrum graphs through software to form a 3D spectrum graph.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116818761A (en) * | 2023-08-16 | 2023-09-29 | 国检中心深圳珠宝检验实验室有限公司 | Method and equipment for detecting color cause of single crystal color precious stone |
| CN116818761B (en) * | 2023-08-16 | 2024-04-19 | 国检中心深圳珠宝检验实验室有限公司 | Method and equipment for detecting color cause of single crystal color precious stone |
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| 李倩，李文宣: "合成及改色钻石的鉴定特征", 宝石和宝石学杂志, vol. 16, no. 06, 15 December 2014 (2014-12-15), pages 21 - 27 * |
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| CN116818761A (en) * | 2023-08-16 | 2023-09-29 | 国检中心深圳珠宝检验实验室有限公司 | Method and equipment for detecting color cause of single crystal color precious stone |
| CN116818761B (en) * | 2023-08-16 | 2024-04-19 | 国检中心深圳珠宝检验实验室有限公司 | Method and equipment for detecting color cause of single crystal color precious stone |
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