CN115616016A - Electronic probe sample surface conductivity treatment method - Google Patents
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- 239000000523 sample Substances 0.000 title claims abstract description 134
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- 238000004458 analytical method Methods 0.000 abstract description 15
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
Abstract
The application provides an electronic probe sample surface conductivity treatment method, and relates to the field of material analysis. The surface conductivity treatment method of the electronic probe sample comprises the following steps: and arranging the ultrathin two-dimensional material with good conductivity on the surface of the non-conductive sample, drying and carrying out heat treatment to obtain the target sample. According to the electronic probe sample surface conductivity processing method, the signal intensity of the target element in the sample subjected to conductivity processing by the graphene film is obviously higher than that of the sample subjected to carbon film evaporation, so that the peak-to-back ratio of the detected signal can be effectively improved by performing conductivity processing on the surface of the sample by the graphene, and the accuracy of quantitative analysis is further improved.
Description
Technical Field
The application relates to the field of material analysis, in particular to a surface conductivity treatment method for an electronic probe sample.
Background
The electron probe technology is a nondestructive in-situ quantitative analysis means, and can detect the elements from beryllium (4 Be) to uranium (92U). The principle of electron probe quantitative analysis is to detect the net intensity (peak intensity minus background intensity) of the characteristic X-ray of the element to be detected for further conversion into the content of the element. In the field of quantitative analysis of electronic probes, accurate quantitative analysis of trace elements faces a great challenge. In the test process, the characteristic X-ray intensity generated by the trace elements is low, the detected peak clear height is greatly interfered by background signals, and the accuracy of a quantitative result is greatly influenced. Therefore, the improvement of the peak-to-back ratio of the detected signal is crucial to the accurate quantitative analysis of trace elements.
The method for improving the quantitative accuracy of the trace elements mainly aims at improving the accelerating voltage, improving the beam intensity and prolonging the testing time. In a published Chinese patent (publication No. CN 107796841A), a method for analyzing the trace elements of the olivine with high precision adopts high voltage 25 kV and long counting time 120 to 240s to analyze the trace elements in the olivine, so that the detection limit of specific elements is optimized to 10ppm to ppm.
At present, methods for improving the accuracy of quantitative analysis of trace elements mainly focus on the improvement of analysis and test conditions, and research from the perspective of improving carbon films is less. When using an electronic probe to test a non-conductive sample, the surface of the sample must be subjected to conductive carbon plating treatment. At present, a vacuum coating instrument is adopted to evaporate an amorphous carbon film on the surface of a sample in a conductive treatment mode, and the thickness of a standard carbon film is regulated to be 20nm (GB/T15074-2008) in the conventional electronic probe quantitative analysis method. The existence of the carbon film can absorb a part of characteristic X-ray signals generated by the sample, and the absorption effect of the carbon film has great influence on the accuracy of quantitative detection of the trace elements because the strength of the characteristic X-rays generated by the trace elements is not high. For trace elements, a stronger peak signal can be obtained to effectively improve the peak-to-back ratio, so that the accuracy of quantitative analysis is improved.
Therefore, it is important how to maintain good conductivity with reduced carbon film thickness.
Disclosure of Invention
The present application aims to provide a method for treating the surface conductivity of an electronic probe sample to solve the above problems.
In order to achieve the purpose, the following technical scheme is adopted in the application:
a surface conductivity treatment method for an electronic probe sample comprises the following steps:
and arranging the ultrathin two-dimensional material with good conductivity on the surface of the non-conductive sample, drying and carrying out heat treatment to obtain the target sample.
Preferably, the ultra-thin two-dimensional material with good electrical conductivity comprises graphene.
Preferably, the graphene is used for preparing a suspension, and the preparation method of the suspension comprises the following steps:
graphene is dispersed in an organic solvent and then sonicated.
Preferably, the organic solvent comprises ethanol.
Preferably, the non-conductive sample comprises Ga doped ZnO.
Preferably, the drying temperature is between room temperature and 60 ℃ and the drying time is 6-24h.
Preferably, the temperature of the heat treatment is 80-400 ℃ and the time is 2-24h.
Preferably, the non-conductive sample is subjected to a polishing treatment before use.
Preferably, the heat treatment is performed under an inert atmosphere.
Compared with the prior art, the beneficial effect of this application includes:
according to the surface conductivity treatment method of the electronic probe sample, the ultrathin two-dimensional material with good conductivity is arranged on the surface of the non-conductive sample, and the target sample of the ultrathin two-dimensional material with good conductivity on the surface is prepared through drying and heat treatment; the excellent conductivity of the ultrathin two-dimensional material with good conductivity is utilized, the surface of a sample can be ensured to keep good conductivity under a high-energy electron beam, the thickness of the ultrathin two-dimensional material with good conductivity is far smaller than that of a currently used amorphous carbon film with the thickness of 20nm, the absorption of the carbon film on the surface of the sample on sample characteristic X rays can be greatly reduced, the detection signal of an electronic probe on trace elements is improved, the peak-to-back ratio is improved, and the accuracy of a quantitative analysis result is further improved.
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments are briefly described below, and it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope of the present application.
FIG. 1 is an electron probe signal intensity for the Ga element L α peak of a coated graphene film provided in example 1 and an evaporated carbon film provided in comparative example 1;
FIG. 2 is a scanning electron micrograph of a sample without polishing treatment (a) and without polishing treatment (b) as provided in comparative example 2;
fig. 3 is a scanning electron micrograph of graphene provided in comparative example 3 without sonication (a) and without sonication (b);
FIG. 4 is a scanning electron micrograph of a sample which was not heat-treated as provided in comparative example 4;
fig. 5 is a scanning electron micrograph of a sample subjected to heat treatment provided in comparative example 4.
Detailed Description
The term as used herein:
"consisting of 8230%" \8230, preparation "and" comprising "are synonymous. The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of 8230% \8230comprises" excludes any unspecified elements, steps or components. If used in a claim, this phrase shall render the claim closed except for the materials described except for those materials normally associated therewith. When the phrase "consisting of 8230' \8230"; composition "appears in a clause of the subject matter of the claims and not immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the recited range should be interpreted to include ranges of "1 to 4," "1 to 3," "1 to 2 and 4 to 5," "1 to 3 and 5," and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In these examples, the parts and percentages are by mass unless otherwise indicated.
"part by mass" means a basic unit of measure indicating a mass ratio of a plurality of components, and 1 part may represent an arbitrary unit mass, for example, 1g or 2.689 g. If the parts by mass of the component A are a parts and the parts by mass of the component B are B parts, the mass ratio of the component A to the component B is expressed as a: b. alternatively, the mass of the A component is aK and the mass of the B component is bK (K is an arbitrary number, and represents a multiple factor). It is unmistakable that, unlike the parts by mass, the sum of the parts by mass of all the components is not limited to 100 parts.
"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).
A surface conductivity treatment method for an electronic probe sample comprises the following steps:
and arranging the ultrathin two-dimensional material with good conductivity on the surface of the non-conductive sample, drying and carrying out heat treatment to obtain the target sample.
In an alternative embodiment, the ultra-thin two-dimensional material with good electrical conductivity comprises graphene.
Graphene is a two-dimensional structure of a hexagonal honeycomb lattice composed of carbon atoms hybridized by sp2 orbits, has a theoretical thickness of only 0.35 nm, and is the thinnest two-dimensional material at present. The unique structure of the graphene endows the graphene with excellent electrical properties, and the electron mobility at normal temperature is 1.5 multiplied by 104 cm 2 V -1 s -1 It is a transparent conductive material with excellent performance.
In an optional embodiment, the graphene is used as a suspension, and a preparation method of the suspension includes:
graphene is dispersed in an organic solvent and then sonicated.
In an alternative embodiment, the organic solvent comprises ethanol.
In an alternative embodiment, the non-conductive sample comprises Ga doped ZnO.
In an alternative embodiment, the drying is carried out at a temperature of from room temperature to 60 ℃ for a period of from 6 to 24 hours.
Optionally, the drying temperature may be 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃ or any value between room temperature and 60 ℃, and the time may be 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h or any value between 6h and 24h.
In an alternative embodiment, the temperature of the heat treatment is between 80 and 400 ℃ for a period of time between 2 and 24 hours.
Optionally, the temperature of the heat treatment may be any value between 80 ℃, 100 ℃, 200 ℃, 300 ℃, 400 ℃ or 80-400 ℃, and the time may be any value between 2h, 4h, 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h or 2-24h.
In an alternative embodiment, the non-conductive sample is polished prior to use.
In an alternative embodiment, the heat treatment is performed under an inert atmosphere.
Embodiments of the present application will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The embodiment provides a surface conductivity treatment method for an electronic probe sample, which specifically comprises the following steps:
(1) Polishing a 0.1 wt% Ga-doped ZnO sample; the polishing treatment step comprises: firstly, sequentially and coarsely grinding No. 120 and No. 500 sandpaper; secondly, fine grinding 800, 1000 and 2000 abrasive paper in sequence; thirdly, soaking the surface of the flannelette, spraying polishing solution, and placing a sample on the surface of the flannelette for polishing;
(2) Dispersing graphene in ethanol;
(3) Placing the dispersion liquid obtained in the step (2) into an ultrasonic cleaning machine for ultrasonic treatment to prepare a uniform graphene suspension liquid;
(4) Coating the graphene turbid liquid obtained in the step (3) on the surface of the Ga-doped ZnO sample subjected to polishing treatment in the step (1) in a rotating mode, and enabling the graphene to be uniformly distributed on the surface of the sample;
(5) Drying the sample obtained in the step (4), wherein the treatment temperature is as follows: room temperature, treatment time: 24 h;
(6) Carrying out heat treatment on the sample obtained in the step (5), wherein the treatment temperature is 200 ℃ in an argon atmosphere, so that the graphene is in close contact with the surface of the sample, and the treatment time is as follows: 24h.
The treated sample was placed in an electronic probe instrument for analysis. And performing local fine slow scanning on the Ga element by adopting State State analysis. Under the test conditions of 15kV and 20nA, an RAP crystal is used for analyzing an L alpha peak of Ga element, the step size is 0.002A, and the retention time is 0.75 s.
Example 2
The embodiment provides a surface conductivity treatment method for an electronic probe sample, which specifically comprises the following steps:
(1) Polishing a 0.1 wt% Ga-doped ZnO sample by the same method as in example 1;
(2) Dispersing graphene in ethanol;
(3) Placing the dispersion liquid obtained in the step (2) into an ultrasonic cleaning machine for ultrasonic treatment to prepare a uniform graphene suspension liquid;
(4) Coating the graphene turbid liquid obtained in the step (3) on the surface of the Ga-doped ZnO sample subjected to polishing treatment in the step (1) in a rotating mode, and enabling the graphene to be uniformly distributed on the surface of the sample;
(5) Drying the sample obtained in the step (4), wherein the treatment temperature is as follows: 40 ℃, treatment time: 12h;
(6) Carrying out heat treatment on the sample obtained in the step (5), wherein the treatment temperature is 300 ℃ in an argon atmosphere, so that the graphene is in close contact with the surface of the sample, and the treatment time is as follows: 12 h.
The treated sample was placed in an electronic probe instrument for analysis. And performing local fine slow scanning on the Ga element by adopting State State analysis. Under the test conditions of 15kV and 20nA, an RAP crystal is used for analyzing an L alpha peak of Ga element, the step size is 0.002A, and the retention time is 0.75 s.
Example 3
The embodiment provides a surface conductivity treatment method for an electronic probe sample, which specifically comprises the following steps:
(1) Polishing a 0.1 wt% Ga-doped ZnO sample by the same method as in example 1;
(2) Dispersing graphene in ethanol;
(3) Placing the dispersion liquid obtained in the step (2) into an ultrasonic cleaning machine for ultrasonic treatment to prepare a uniform graphene suspension liquid;
(4) Coating the graphene suspension liquid obtained in the step (3) on the surface of the Ga-doped ZnO sample subjected to polishing treatment in the step (1) in a spinning manner, so that graphene is uniformly distributed on the surface of the sample;
(5) Drying the sample obtained in the step (4), wherein the treatment temperature is as follows: 40 ℃, treatment time: 12h;
(6) Carrying out heat treatment on the sample obtained in the step (5), wherein the treatment temperature is 400 ℃ in an argon atmosphere, so that the graphene is in close contact with the surface of the sample, and the treatment time is as follows: and 2h.
The treated sample was placed in an electronic probe instrument for analysis. And performing local fine slow scanning on the Ga element by adopting State State analysis. Under the test conditions of 15kV and 20nA, an RAP crystal is used for analyzing an L alpha peak of Ga element, the step size is 0.002A, and the retention time is 0.75 s.
Comparative example 1
The sample tested in example 1 was taken out of the electron probe and polished, and the polished Ga-doped ZnO sample was subjected to carbon film deposition treatment, wherein the thickness of the carbon film on the surface of the sample was 20 nm.
The sample after the carbon film evaporation treatment is placed in an electronic probe instrument for analysis, the same parameters as those in example 1 are selected, and the fine slow scanning is performed on the Ga L alpha peak.
Fig. 1 shows the signal intensity of the electronic probe of the trace element Ga element L α peak, and the result shows that the signal intensity of the Ga element in the sample subjected to the conductive treatment by using the graphene film is significantly higher than the signal intensity of the sample subjected to the vapor deposition carbon film treatment, so that the peak-to-back ratio of the detected signal can be effectively improved by performing the conductive treatment on the sample surface by using the graphene, and the accuracy of the quantitative analysis can be further improved.
Comparative example 2
Unlike example 1, no polishing treatment was performed.
In FIG. 2, a is a scanning electron micrograph of the unpolished sample surface, and the results show that the unpolished sample surface is uneven and not suitable for electron probe test; in fig. 2, b is a scanning electron microscope image of the polished sample surface, and the result shows that the polished sample surface is flat and suitable for the electronic probe test.
The surface of a sample which is not polished is uneven, the uneven surface plays a role in scattering incident electron beams, emergent X rays are subjected to irregular absorption, the signal intensity is reduced, the accuracy of a test result is influenced, and the method is not suitable for component analysis of an electron probe; the polished sample has smooth surface, and the sample surface can not interfere incident electron beams and emergent X rays, so that the method is suitable for component analysis of the electron probe.
Comparative example 3
Unlike example 1, graphene was not sonicated.
In fig. 3, a is a scanning electron microscope image without ultrasonic treatment, and the result shows that the graphene clusters are seriously agglomerated on the surface of the sample when the graphene powder dispersed in ethanol is not subjected to ultrasonic treatment; in fig. 3, b is a scanning electron microscope image of the graphene sheet after ultrasonic treatment on the surface of the sample, and the result shows that the graphene sheet with good dispersibility is spread and spread on the surface of the sample.
The graphene cluster is multilayer graphene, the thickness is large, the absorption effect on characteristic X-ray signals is serious, the received signals of the detector are reduced, and the accuracy of a test result is influenced; the graphene sheet with good dispersibility is spread and paved on the surface of a sample, the absorption effect of the thin-layer graphene on the characteristic X-ray is small, the peak-to-back ratio of a detection signal can be effectively improved, and the accuracy of an analysis result is improved.
Comparative example 4
Unlike example 1, the heat treatment of the step (6) was not performed.
FIG. 4 is a scanning electron microscope image of a sample without heat treatment, wherein the surface of the sample is firstly subjected to scanning electron microscope shooting for 1 time (FIG. 4, a), and 2 times of shooting are carried out after 5 seconds (FIG. 4, b), and the two shooting results are compared, so that the position of the sample is found to generate drift, and the sample is proved to have poor conductivity and be not suitable for electron probe analysis; FIG. 5 is a scanning electron microscope image of a sample after heat treatment, wherein the surface of the sample is firstly photographed 1 time by a scanning electron microscope (FIG. 5, a), and 2 times of photographing are carried out after 5 seconds (FIG. 5, b), and the results of the two photographing are compared, so that the sample is found to have no drift in position, and the sample has good conductivity and is suitable for electronic probe test analysis.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit the same; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.
Moreover, those of skill in the art will understand that although some embodiments herein include some features included in other embodiments, not others, combinations of features of different embodiments are meant to be within the scope of the application and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the application and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (9)
1. A surface conductivity treatment method for an electronic probe sample is characterized by comprising the following steps:
and arranging the ultrathin two-dimensional material with good conductivity on the surface of the non-conductive sample, drying and carrying out heat treatment to obtain the target sample.
2. The method for processing the surface conductivity of the electronic probe sample according to claim 1, wherein the ultra-thin two-dimensional material with good conductivity comprises graphene.
3. The method for processing the surface conductivity of the electronic probe sample according to claim 2, wherein the graphene is used as a suspension, and the method for preparing the suspension comprises:
graphene is dispersed in an organic solvent and then sonicated.
4. The method according to claim 3, wherein the organic solvent comprises ethanol.
5. The method of claim 1, wherein the non-conductive sample comprises Ga-doped ZnO.
6. The method for processing the surface conductivity of the electronic probe sample according to claim 5, wherein the drying temperature is from room temperature to 60 ℃ and the drying time is from 6 to 24 hours.
7. The method for processing the surface conductivity of the electronic probe sample according to claim 5, wherein the temperature of the heat treatment is 80-400 ℃ and the time is 2-24h.
8. The method of claim 1, wherein the heat treatment is performed under an inert atmosphere.
9. The method for treating the surface conductivity of the electronic probe sample according to any one of claims 1 to 8, wherein the non-conductive sample is subjected to polishing treatment before use.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010059525A (en) * | 2008-09-08 | 2010-03-18 | Jeol Ltd | Carbon vapor deposition system |
| CN102353817A (en) * | 2011-06-30 | 2012-02-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Probe of conducting atomic force microscope and measuring methods employing probe |
| GB201222559D0 (en) * | 2012-12-14 | 2013-01-30 | Univ Barcelona Autonoma | Conductive atomic force microscope tips coated with graphene |
| CN103864062A (en) * | 2014-01-27 | 2014-06-18 | 沈阳大学 | Preparation method of graphene transparent conductive film |
| KR101608681B1 (en) * | 2014-11-14 | 2016-04-04 | 서울대학교산학협력단 | Non-destructive method for obtaining electron microscopy image and non-destructive analyzing method |
| CN105648415A (en) * | 2015-12-31 | 2016-06-08 | 中国地质大学（武汉） | Sample stand of film coater |
| CN106744841A (en) * | 2016-12-21 | 2017-05-31 | 广东工业大学 | A kind of preparation method of the three-dimensional porous graphene film that single-layer graphene is constructed |
| CN110093645A (en) * | 2019-05-31 | 2019-08-06 | 厦门大学 | Plastic electroplating method |
-
2022
- 2022-12-14 CN CN202211597976.2A patent/CN115616016A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010059525A (en) * | 2008-09-08 | 2010-03-18 | Jeol Ltd | Carbon vapor deposition system |
| CN102353817A (en) * | 2011-06-30 | 2012-02-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Probe of conducting atomic force microscope and measuring methods employing probe |
| GB201222559D0 (en) * | 2012-12-14 | 2013-01-30 | Univ Barcelona Autonoma | Conductive atomic force microscope tips coated with graphene |
| CN103864062A (en) * | 2014-01-27 | 2014-06-18 | 沈阳大学 | Preparation method of graphene transparent conductive film |
| KR101608681B1 (en) * | 2014-11-14 | 2016-04-04 | 서울대학교산학협력단 | Non-destructive method for obtaining electron microscopy image and non-destructive analyzing method |
| CN105648415A (en) * | 2015-12-31 | 2016-06-08 | 中国地质大学（武汉） | Sample stand of film coater |
| CN106744841A (en) * | 2016-12-21 | 2017-05-31 | 广东工业大学 | A kind of preparation method of the three-dimensional porous graphene film that single-layer graphene is constructed |
| CN110093645A (en) * | 2019-05-31 | 2019-08-06 | 厦门大学 | Plastic electroplating method |
Non-Patent Citations (1)
| Title |
|---|
| 王悦 等: "《石墨烯基电极材料研究进展》" * |
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