CN112903733B - Transmission electron microscope energy spectrum super-resolution analysis method - Google Patents
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Abstract
The invention provides a transmission electron microscope energy spectrum super-resolution analysis method, belonging to the fields of mineral resource exploration and trace element geochemistry. The method comprises the following steps: step 1, selecting and analyzing a target sample. And 2, preparing a micro-area trace element composition analysis sample. And 3, analyzing the properties and the element composition of the target sample. And 4, preparing a transmission electron microscope observation sample according to the requirement. And 5, placing the prepared sample in the last step into a transmission electron microscope for appearance observation, and searching a proper analysis position. The invention can detect trace elements of a sample under the nanoscale, greatly improves the practical application detection limit of the transmission electron microscope energy spectrum element analysis, also provides a solution for the interference of the trace elements in the sample by the signal of the main element, and can also be applied to the energy spectrum analysis of an electron beam sensitive sample.
Description
Technical Field
The invention belongs to the field of mineral resource exploration and chemical detection of trace elements, and particularly relates to a transmission electron microscope energy spectrum super-resolution analysis method.
Background
The key metal has the characteristics of being thin, accompanied and fine, and is usually present in the ore minerals in the forms of tiny minerals, similar images, adsorbed ions and the like. The occurrence state of the key metal elements in the ore minerals can be cleared up, so that not only can important data be provided for the research of the ore deposit, but also an important basis for improving the efficient and clean utilization level of the key technical elements is provided.
At present, in micron and submicron scale, the identification of the occurrence state of trace elements in mineral rocks is mostly carried out by using electron probes, LA-ICP-MS, secondary ion mass spectrometry and other micro-area analysis equipment, and the scale thereof is mostly applied to a transmission electron microscopy analysis platform. The transmission electron microscope has powerful functions and plays an important role in the field of nano-geoscience research, whereinMost of the element analysis modules of the transmission electron microscope are energy spectrometers, and the resolution (125ev) of the energy spectrometers is low and easy to overlap, so that the spectral peak of the main quantity element generates strong interference to the spectral peak of the trace element. In addition, the detection limit of the spectrometer (theoretical detection limit 0.1-0.5%) is also difficult to meet in trace element analysis. The content of trace elements such as rare earth elements as strategic elements in the mineral is several hundred ppm (10) -6 ). For example, the ion-adsorbing rare earth deposit in China supplies more than 90% of heavy rare earth elements in the world, and the rare earth elements of the deposit mostly exist on particulate minerals (less than 2um), but further in the research of nanometer scale, because the actual detection limit of elements of the energy spectrum of a transmission electron microscope is difficult to meet the requirement, the research faces obstruction; the phosphorite type rare earth deposit has rare earth elements existing in nano apatite, but the rare earth elements can not be detected by conventional energy spectrum detection in nano-scale research, so that the rare earth element existence research of the deposit is difficult to carry out.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a transmission electron microscope energy spectrum super-resolution analysis method.
The invention adopts the following technical scheme:
the invention provides a transmission electron microscope energy spectrum super-resolution analysis method, which comprises the following steps:
step 1, selecting and analyzing a target sample;
step 2, preparing a trace element composition analysis sample;
step 3, analyzing the property and element composition of the target sample (whether the sample is an electron beam sensitive sample, and the composition of the main element and the target trace element of the sample);
step 4, preparing a transmission electron microscope observation sample according to the requirement;
step 6, inquiring the peak position of an X-ray photoelectron spectrometer of related elements, mainly distinguishing main elements possibly interfering with the peak position of the target trace element, and searching key peak positions of the trace elements which can be distinguished from the peak position of the main element energy spectrum;
and 7, aiming at the trace element detection requirement, the traditional STEM mode is not adopted for energy spectrum analysis, but the TEM mode is adopted for energy spectrum signal acquisition in the parallel light mode, so that the energy spectrum signal acquisition amount is greatly improved, and the purpose of trace element analysis in the nanometer scale is achieved.
The step (1) specifically comprises the following steps: identifying basic classifications of mineral rocks by eye and microscope; determining the types and the contents of the trace elements of the target sample by a corresponding chemical analysis method according to the types of the mineral rocks; after the chemical analysis is completed, the mineral rock containing the trace elements reaching the ore grade is selected as the target sample.
The method for identifying the mineral phase, observing the morphology and analyzing the element composition in the step (3) comprises but is not limited to the following microscopic equipment which can be used for analyzing the surface morphology of the sample; micro-area X-ray diffraction method (micro-area beam spot is usually less than 100 microns), powder X-ray diffraction method, optical microscope, scanning electron microscope, atomic force microscope, ICP-OES, ICP-MS, electron probe, electron energy spectrum, laser ablation-inductively coupled plasma mass spectrum, secondary ion mass spectrum method.
Using an optical microscope to finish the appearance observation of the minerals under the micron scale of the rock slices and the distribution characteristics of macroscopic minerals;
the research on the appearance, distribution relation and element composition of minerals at micron scale is completed by a scanning electron microscope;
laser ablation-inductively coupled ion mass spectrometry LA-ICP-MS is used for detecting the content of trace elements of minerals in situ on a micrometer scale;
The method is completed by secondary ion mass spectrometry SIMS and is used for detecting the content of trace elements of minerals in situ at a micrometer scale. The analysis method in the step (7) mainly comprises the following steps: firstly, under a TEM (transmission electron microscope) parallel light mode, long-time characteristic X-ray signal acquisition is carried out on a target area, and the counting of energy spectrum signals can be greatly improved, so that the analysis of target trace elements is realized;
analyzing the element composition of the sample according to the peak positions of the main element and the trace element, and searching the peak position of the trace element which does not overlap with the peak position of the main element;
thirdly, according to the analysis area with a special shape, the shape of the light spot can be changed by adjusting a C2 mirror of the transmission electron microscope to acquire energy spectrum signals;
and fourthly, aiming at the electron beam sensitive sample, the current intensity can be properly reduced, the diameter of a light spot is enlarged, and the energy spectrum signal acquisition is carried out.
The invention has the beneficial effects that:
the invention can detect the trace elements of the sample under the nanometer scale, greatly improves the practical application detection limit of the energy spectrum analysis of the transmission electron microscope, also provides a solution for the interference of the trace elements in the sample by the signal of the main element, and can also be applied to the energy spectrum analysis of the electron beam sensitive sample. According to the steps of the invention, certain steps can be skipped to carry out any combination according to the sequence from front to back according to the actual requirements.
(1) The invention provides a super-resolution analysis method for a transmission electron microscope energy spectrum, which can greatly improve the element detection efficiency of the transmission electron microscope energy spectrum and provide help for trace element analysis in nano scientific research.
(2) The invention provides a solution for the problems of low element content, interference of main element elements, analysis of element content of electron beam sensitive samples and the like in the research of occurrence states of key metal elements, and provides a basic guarantee for improving the development and utilization level of a plurality of key metal mineral resources which are difficult to select and extract.
(3) The method has the advantages of analyzing chemical elements in the transmission electron microscope research geoscience sample, because the geoscience sample is mostly an electron beam sensitive sample, and the method can protect the sample to the maximum extent and reduce the damage of the electron beam to the sample.
Drawings
FIG. 1 is a high resolution TEM image of nano apatite particles taken in TEM mode;
FIG. 2 is a graph showing apatite particle dotting energy spectrum of FIG. 1 in STEM mode, which is a conventional detection means;
FIG. 3 is a TEM mode of transmission electron microscope, the apatite particle dotting energy spectrum in FIG. 1;
FIG. 4 is an enlarged view of the pink frame of FIG. 3;
FIG. 5 is a flow chart of the steps of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described below clearly and completely, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 5, the present invention provides a transmission electron microscope energy spectrum super-resolution analysis method, which comprises the following steps:
step 1, selecting and analyzing a target sample;
step 2, preparing a trace element composition analysis sample;
step 3, analyzing the property and element composition of the target sample (whether the sample is an electron beam sensitive sample, and the composition of the main element and the target trace element of the sample);
step 4, preparing a transmission electron microscope observation sample according to the requirement;
step 6, inquiring the peak position of an X-ray photoelectron spectrometer of related elements, mainly distinguishing main elements possibly interfering with the peak position of the target trace element, and searching key peak positions of the trace elements which can be distinguished from the peak position of the main element energy spectrum;
And 7, aiming at the trace element detection requirement, the traditional STEM mode is not adopted for energy spectrum analysis, but the TEM mode is adopted for energy spectrum signal acquisition in the parallel light mode, so that the energy spectrum signal acquisition amount is greatly improved, and the purpose of trace element analysis in the nanometer scale is achieved.
The step (1) specifically comprises the following steps: identifying basic classifications of mineral rocks by eye and microscope; determining the types and the contents of the trace elements of the target sample by a corresponding chemical analysis method according to the types of the mineral rocks; after completion of the chemical analysis, the mineral rock containing the trace element of interest is selected as the target sample.
The method for identifying the mineral phase, observing the morphology and analyzing the element composition in the step (3) comprises but is not limited to the following microscopic equipment which can be used for analyzing the surface morphology of the sample; micro-area X-ray diffraction method (micro-area beam spot is usually less than 100 microns), powder X-ray diffraction method, optical microscope, scanning electron microscope, atomic force microscope, ICP-OES, ICP-MS, electron probe, electron energy spectrum, laser ablation-inductively coupled plasma mass spectrum, secondary ion mass spectrum method.
The analysis method in the step (7) mainly comprises the following steps: firstly, under a TEM (transmission electron microscope) parallel light mode, long-time characteristic X-ray signal acquisition is carried out on a target area, and the counting of energy spectrum signals can be greatly improved, so that the analysis of target trace elements is realized;
Analyzing the element composition of the sample according to the peak positions of the main elements and the trace elements, and searching the peak position of the trace element which does not overlap with the peak position of the main elements;
thirdly, according to the analysis area with a special shape, the shape of the light spot can be changed by adjusting a C2 mirror of the transmission electron microscope to collect energy spectrum signals;
and fourthly, aiming at the electron beam sensitive sample, the current intensity can be properly reduced, the diameter of a light spot is enlarged, and the energy spectrum signal acquisition is carried out.
Examples
The transmission electron microscope is widely applied in the fields of nano-geoscience, material science and the like, and is an important tool for research on a nano scale due to the ultrahigh spatial resolution. FIG. 1 is a high-resolution TEM image of nano apatite particles taken in TEM mode of TEM, which can clearly show the morphology and structure of the particles and shows the advantages of TEM for studying nano minerals.
This example illustrates the identification of the rare earth element Y of the isomorphism in apatite, on the one hand, it is found by LA-ICP-MS that the content of rare earth element is about 600ppm (0.06 wt%), while the theoretical detection limit of the energy spectrum is 0.1-0.5 wt%; on the other hand, the Y element is usually discriminated by the discrimination peak position L α of 1.92Kev, while the K peak position of the principal component element P of 2.02Kev differs from the discrimination peak position L α of 0.1Kev and is lower than the energy resolution of the spectrum of 0.13Kev, so that it cannot be discriminated and hence it is necessary to discriminate by the Y element K peak of 14.93 Kev.
Referring to fig. 2 and 4, fig. 2 is a graph showing the apatite particle dotting energy spectrum of fig. 1 in a STEM mode by using a conventional detection means, and fig. 4 is a graph showing the apatite particle dotting energy spectrum of fig. 1 in a TEM mode by using a transmission electron microscope. By comparison of the energy spectrum counts of the conventional method and the method of the present invention, the method of the present invention is 1.5 ten thousand times that of the conventional method. By comparing fig. 3 and fig. 5, fig. 3 is an enlarged view of energy position of 13.5KeV-16.5KeV in fig. 2, and fig. 5 is an enlarged view of energy position of 13.5KeV-16.5KeV in fig. 4, it can be seen that the method of the present invention can well detect the signal of Y element in apatite, and realize the analysis and detection of trace element Y element, while the conventional dotting analysis method can not meet the requirement.
When the STEM dotting analysis time is tried to be increased, a natural sample is relatively unstable due to the fact that a transmission sample is thin, breakdown can be caused in a short time, and the sample is damaged; secondly, a higher signal quantity cannot be acquired. When an attempt is made to compare the analysis with STEM-Mapping, a high count can be obtained even by long-time Mapping, but the time taken is about 10 times that of the method of the present invention, and the efficiency is low.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A super-resolution analysis method for energy spectrum of a transmission electron microscope is characterized by comprising the following steps:
step 1, selecting and analyzing a target sample;
step 2, preparing a micro-area trace element composition analysis sample;
step 3, analyzing the property and element composition of the target sample;
mainly judging whether the sample is an electron beam sensitive sample or not, wherein the sample consists of main elements and target trace elements;
the property analysis method of the sample in the step 3 specifically comprises the following steps:
using an optical microscope to finish the appearance observation of the rock slice on minerals under the micron scale and the distribution characteristics of macroscopic minerals;
the research on the appearance, distribution relation and element composition of minerals at micron scale is completed by a scanning electron microscope;
laser ablation-inductively coupled ion mass spectrometry LA-ICP-MS is used for detecting the content of trace elements of minerals in situ on a micrometer scale;
secondary ion mass spectrum SIMS is used for detecting the content of trace elements of minerals in situ at a micrometer scale;
step 4, preparing a transmission electron microscope observation sample according to the requirement;
step 5, placing the sample prepared in the previous step into a transmission electron microscope, carrying out morphology observation under the nanoscale, and searching a proper analysis position;
Step 6, looking up the peak position of an X-ray photoelectron spectrometer of related elements, mainly distinguishing the main elements interfering with the peak position of the target trace element, and searching the key peak position of the trace element which can be distinguished from the peak position of the energy spectrum of the main elements;
step 7, aiming at the detection requirement of the trace elements, a TEM mode is adopted to collect energy spectrum signals in a parallel light mode, so that the energy spectrum signal counting is greatly improved, and the purpose of analyzing the trace elements in a nanoscale is achieved;
according to the size and the shape of a target area of a detection sample, the size and the shape of a light spot are changed by adjusting a C2 mirror of a transmission electron microscope;
the detection of the trace elements comprises the following specific operations:
under a TEM (transmission electron microscope) parallel light mode, long-time characteristic X-ray signal acquisition is carried out on a target area, so that the counting of energy spectrum signals can be greatly improved, and the analysis of target trace elements is realized;
aiming at the element composition of the sample, analyzing according to the peak positions of the major elements and the trace elements, and searching the peak position of the trace element which does not overlap with the peak position of the major elements; according to the analysis region with a special shape, the shape of a light spot is changed by adjusting a C2 mirror of the transmission electron microscope to acquire energy spectrum signals;
Aiming at an electron beam sensitive sample, reducing the current intensity and enlarging the diameter of a light spot to acquire an energy spectrum signal;
the method is applied to the identification of the isomorphism rare earth element Y in the apatite, and the content of the rare earth element is 600 ppm.
2. The transmission electron microscope energy spectrum super-resolution analysis method according to claim 1, wherein the step 1 specifically comprises the following steps:
identifying basic classifications of mineral rocks by eye and microscope;
determining the types and the contents of the trace elements of the target sample by a corresponding chemical analysis method according to the types of the mineral rocks;
after the chemical analysis is completed, the mineral rock containing the trace elements reaching the ore grade is selected as a target sample.
3. The transmission electron microscopy energy spectrum super-resolution analysis method according to claim 1, characterized in that element composition analysis is performed by adopting one or any combination of ICP-OES, ICP-MS, electron probe, electron energy spectrum, laser ablation-inductively coupled ion mass spectrometry and secondary ion mass spectrometry in step 3.
4. The super-resolution analysis method for transmission electron microscopy spectroscopy as set forth in claim 1, wherein the analysis method for mineral phase composition in step 3 is selected from the group consisting of a micro-area X-ray diffraction method and a powder X-ray diffraction method.
5. The method for super-resolution analysis of transmission electron microscopy energy spectrum according to claim 1, wherein the method for preparing the transmission electron microscopy observation sample in the step 4 comprises: a powder sample preparation method, an ultrathin section method, an ion thinning method and a focused ion beam sample preparation method, and a transmission sample with the thickness of less than 100nm is obtained.
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| CA1212783A (en) * | 1983-10-28 | 1986-10-14 | George M. Bancroft | Suppression of molecular ions in secondary ion mass spectra |
| WO2009046392A1 (en) * | 2007-10-04 | 2009-04-09 | Trustees Of Princeton University | Synthesis of bio-functionalized rare earth doped upconverting nanophosphors |
| CN107629792B (en) * | 2017-09-30 | 2021-01-15 | 华南师范大学 | Up-conversion super-resolution imaging nano probe and preparation method and application thereof |
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| WO2011099434A1 (en) * | 2010-02-12 | 2011-08-18 | 独立行政法人産業技術総合研究所 | Standard sample for determination of detection sensitivity of elemental analyzer attached to transmission electron microscope |
| CN104181175A (en) * | 2014-07-18 | 2014-12-03 | 中山大学 | Water particle geochemical prospecting method and application thereof |
| EP3121834A1 (en) * | 2015-07-23 | 2017-01-25 | FEI Company | Fiducial formation for tem/stem tomography tilt-series acquisition and alignment |
| CN106480195A (en) * | 2016-10-21 | 2017-03-08 | 中国科学院地质与地球物理研究所 | The method that the combination of fluorescent electronic microscope is identified to microorganism and mineralising is analyzed |
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