CN114088751B - Multilayer film transmission electron microscope sample and preparation method thereof - Google Patents
Multilayer film transmission electron microscope sample and preparation method thereof Download PDFInfo
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- CN114088751B CN114088751B CN202111343001.2A CN202111343001A CN114088751B CN 114088751 B CN114088751 B CN 114088751B CN 202111343001 A CN202111343001 A CN 202111343001A CN 114088751 B CN114088751 B CN 114088751B
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005498 polishing Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000010432 diamond Substances 0.000 claims abstract description 11
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 11
- 239000010408 film Substances 0.000 claims description 47
- 244000137852 Petrea volubilis Species 0.000 claims description 21
- 238000005520 cutting process Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000003292 glue Substances 0.000 claims description 8
- 239000004848 polyfunctional curative Substances 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 7
- 230000003287 optical effect Effects 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 8
- 238000005464 sample preparation method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000004544 sputter deposition Methods 0.000 abstract description 5
- 238000010894 electron beam technology Methods 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 description 13
- 239000012188 paraffin wax Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 235000010585 Ammi visnaga Nutrition 0.000 description 1
- 244000153158 Ammi visnaga Species 0.000 description 1
- 101100008044 Caenorhabditis elegans cut-1 gene Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
Classifications
-
- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention discloses a transmission electron microscope sample of a multilayer film and a preparation method thereof, wherein the transmission electron microscope sample comprises: aiming at the difficulties that the thicknesses of different film layers are uneven in the conventional preparation process of the multi-layer film transmission electron microscope sample, the invention adopts the wedge-shaped transmission electron microscope sample preparation method, can prepare the transmission electron microscope sample with flat surface, uniform thickness of the substrate and each film layer and large-area thin area. The method is suitable for preparing multi-layer film materials except diamond, can reduce the thickness of the sample to the thickness through which electron beams can penetrate through mechanical polishing, or can reduce the sample to the thickness through which electrons can penetrate through only by ion thinning for a short time, can obviously reduce the preferential sputtering phenomenon in the ion thinning process, and can realize a wider scope of electron microscope observation areas.
Description
Technical Field
The invention belongs to the technical field of electron microscope sample preparation, and particularly relates to preparation of a large-area flat thin-area sample.
Background
The transmission electron microscope sample preparation technology is a key ring in the transmission electron microscope microstructure research, and is also a decisive factor in the whole transmission electron microscope microstructure observation. The transmission electron microscope photograph and the spectrogram quality are directly proportional to the sample quality. Depending on the nature of the material, how much material is, and the purpose of the experiment, various sample preparation methods have been devised, such as: mechanical thinning, electrolytic double spraying, ultra-thin slicing, crushing grinding, ion thinning, focused Ion Beam (FIB) thinning, and the like. The traditional sample preparation method has the advantages of small sample thin area, uneven sample and obvious preferential sputtering phenomenon. FIB techniques can achieve surface leveling, but at higher cost and with smaller thin regions. The sample preparation method generally chosen generally requires that the structure of the material intended to be observed or measured is not affected, that the sample prepared must be electronically transparent, that it be thin and uniform (generally, the thinner the better) and that it be stable under electron beams.
Disclosure of Invention
In view of the characteristics of high hardness, low toughness, difficult processing and the like of glass or quartz substrates, the deep research on a sample processing technology suitable for TEM characterization is needed, and the guarantee is provided for obtaining high-quality STEM and HRTEM pictures. Compared with the traditional sample preparation method, the Tripod polishing method can reduce the thickness of the sample to the thickness through which the electron beam can penetrate through mechanical polishing, or the sample can be thinned to the thickness through which the electron beam can penetrate through the sample only by ion thinning in a short time, so that the preferential sputtering phenomenon in the ion thinning process can be remarkably reduced
The invention is realized by the following technical scheme.
In particular to a preparation method of a transmission electron microscope sample of a multilayer film, which comprises the following steps:
1) Cutting pretreatment: cutting the film into long strips, soaking in a solvent, wiping the film clean, and removing the solvent on the surface of the film;
2) And (3) sticking: mixing a hardener with resin to obtain G1 glue, smearing the G1 glue on the surfaces of the cut and treated films, attaching the surfaces of the two films together, and baking and curing;
3) Cutting again: cutting the cured sample into a plurality of thin slices along the normal direction;
4) Mechanical polishing: adhering the cut sample to a sample stage, placing the sample stage on a rotary table, and polishing two sides of the sample in a grading manner; polishing the sample step by adopting different sand papers, and separating the sample from a sample table to finish the mechanical thinning of the transmission electron microscope sample;
5) Ion thinning:
and simultaneously thinning the two sides, controlling voltage to thin each side, and obtaining the transmission electron microscope sample of the multilayer film, wherein the thin thickness of the sample is below 0.1 micrometer.
Preferably, the surface is further wiped clean under an optical microscope by dipping in acetone, and finally the acetone on the surface of the film is removed by alcohol.
Preferably, the hardener is mixed with the resin in a mass ratio of (1-3) (8-12).
Preferably, the hardener is a polyamide hardener 650, 651.
Preferably, the step of polishing the sample comprises the steps of firstly using 100-mesh diamond sand paper, and replacing diamond particles with 500-1000-mesh sand paper after the surface of the sample is ground; finally polishing with sand paper of 0.5 μm or 0.1 μm, and finishing the first surface polishing after confirming no scratch; and then polishing the second surface, and determining different sand paper and rotating speeds according to different thicknesses.
Preferably, the method for determining different sand paper and rotating speed according to different thicknesses comprises the steps of using 200-mesh sand paper with the thickness of 500 micrometers and the rotating speed of 800-1000r/min; 1000-mesh sand paper is used for 100 micrometers in thickness, and the rotating speed is 600-800r/min.
Preferably, the sample is cut using a diamond wire cutting machine.
Preferably, the control voltage is 100-500-Kev, and each side is thinned for 3-5min.
The transmission electron microscope sample of the multilayer film prepared by the method.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1) In the process of preparing the sample by adopting the wedge-shaped sample preparation method, a precise wire cutting machine is firstly used for cutting a larger sample to reduce the thickness and depth of damage. In the specific grinding and polishing process, two-sided polishing is adopted, and sand paper with the particle size of 0.1um is adopted for polishing the film in the later stage. The method can reduce the thickness of the thin film region to below 1um by a mechanical grinding mode, only needs a short-time ion thinning process in the later stage, can obviously improve the preferential sputtering phenomenon in the ion thinning process caused by the difference of the substrate and different film materials, ensures that a thin film sample has a uniform and flat large-area thin region, reduces the damage introduced in the sample cutting and thinning process, and ensures the reality and reliability of the subsequent TEM characterization.
2) The Tripod method can realize the preparation of a large-area flat thin-area TEM sample, and is suitable for representing microscopic mechanisms between film layers and between a film and a substrate.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate and do not limit the invention, and together with the description serve to explain the principle of the invention:
FIG. 1 is a high-foot annular dark field image of a laser speckle-larger multilayer thin film transmission electron microscope sample prepared in example 1;
FIG. 2 is a high-foot annular dark field image of a laser speckle-reduced multilayer thin film transmission electron microscope sample prepared in example 2.
Detailed Description
The present invention will now be described in detail with reference to the drawings and the specific embodiments thereof, wherein the exemplary embodiments and descriptions of the present invention are provided for illustration of the invention and are not intended to be limiting.
The invention discloses a method for preparing carbon nanotubes from coal, which comprises the following steps:
1) Cutting:
according to the characteristics of the multilayer film, firstly, a diamond wire saw is adopted to cut the film into long strips with the width of 2mm, then, the cut blocks are soaked in acetone to remove impurities or pollutants such as paraffin, then, a cotton swab dipped with acetone is used to wipe the surface of the film clean under an optical microscope, and finally, alcohol is used to remove the acetone on the surface of the film.
2) And (3) sticking:
firstly, the hardener polyamide curing agent 650, 651 (yellow) of the G1 glue and the resin (white) are weighed and fully mixed according to the mass ratio of (1-3) (8-12), then, a small amount of the prepared G1 glue is smeared on the surfaces of the films which are cut and treated cleanly by using a pin or toothpick, and then, the two films are attached together in a surface-to-surface mode. The film sample, which was well adhered, was then placed in a spring holder and then in an oven and baked at 130 c for two hours to cure.
3) Cutting again:
when the temperature of the opposite-sticking sample is reduced to room temperature, the sample is taken out, and the sample is cut into a plurality of thin slices with the thickness of about 1mm along the normal direction by a diamond wire saw.
4) Mechanical polishing:
the cut sample was glued to the sample stage with paraffin at 130 c and then the micrometer on the Tripod was adjusted so that the sample and the two supporting columns were in the same horizontal plane. After the Tripod sample stage was prepared, the Tripod sample stage was placed on the turntable to begin polishing the sample. The sample stage is placed on a turntable to polish the two sides of the sample in stages.
In general, firstly, 100-mesh diamond sand paper is used, and after the surface of a sample is ground, the diamond particles are replaced by 500-1000-mesh sand paper; finally, after polishing with 0.5um or 0.1um sandpaper and checking with an optical microscope to confirm that there is no scratch, the first side is considered to be polished. And then taking down the sample table, placing the sample table on a hot table to liquefy the paraffin, taking down the sample, and then adhering the turnover surface of the sample on the sample table again by using the paraffin to polish the second surface.
Before polishing the second side, the height of the support column (typically about 500 um) is increased by a micrometer to be greater than the sample plane height. When the second surface is polished, different sand paper and rotating speeds are needed under different thicknesses, so that the use of an optical microscope to timely measure the thickness change of the sample is very important. Comprises the steps of using 200-mesh sand paper with the thickness of 500 micrometers and the rotating speed of 800-1000r/min; 1000-mesh sand paper is used for 100 micrometers in thickness, and the rotating speed is 600-800r/min. Thinning the sample to the edge resulted in interference fringes. Finally, the final polishing was performed with 0.5um or 0.1um sandpaper. Next we cut a molybdenum ring with an inner diameter of 1.5mm and cut 1/3, then glue the molybdenum ring to the sample with AB glue, after which it was put into acetone together with the sample column (paraffin removed). After about 20 minutes, the sample and the sample stage are automatically separated. The mechanical thinning process of the transmission electron microscope sample is completed.
5) Ion thinning:
in general, mechanically thinned samples remain thicker or have limited thin regions. Ion thinning is required. When the ions are thinned, the two sides are thinned simultaneously. The lower voltage is used, the thinning time is about a few minutes, and the final thinning requires the use of an ultralow voltage (500-100K eV). Because the sample is thin after the mechanical thinning is finished by using the Tripod method, the total ion thinning time is generally within 10 minutes, so that adverse effects such as ion damage and preferential sputtering of different film layers in the multilayer film can be remarkably reduced.
Specific examples are given below to further illustrate the invention.
Example 1:
the method adopts the processes of cutting, opposite sticking, mechanical polishing, ion thinning and the like, and adopts the wedge-shaped transmission electron microscope sample preparation technology to obtain a large-area flat thin area aiming at a multilayer film sample with larger laser speckle. The microstructure of different film layers, between film layers and between film and substrate can be clearly studied. As shown in the electron microscope results of fig. 1, the thickness of the first film grown on the substrate is relatively thin.
FIG. 1 is a high-foot annular dark field image of a prepared multilayer thin film transmission electron microscope sample, and different film layers can be seen to be even and flat from the figure.
Example 2:
the method comprises the steps of cutting, opposite-sticking, mechanical polishing, ion thinning and the like, and a large-area flat thin area is obtained by utilizing a wedge-shaped transmission electron microscope sample preparation technology aiming at a multilayer film sample with smaller laser speckles. The microstructure of different film layers, between film layers and between film and substrate can be clearly studied. As shown in the electron microscope results of fig. 2, the thickness of the first film grown on the substrate was thicker.
The invention is not limited to the above embodiments, and based on the technical solution disclosed in the invention, a person skilled in the art may make some substitutions and modifications to some technical features thereof without creative effort according to the technical content disclosed, and all the substitutions and modifications are within the protection scope of the invention.
Claims (7)
1. The preparation method of the transmission electron microscope sample of the multilayer film is characterized by comprising the following steps:
1) Cutting pretreatment: cutting the film into long strips, soaking in a solvent, wiping the film clean, and removing the solvent on the surface of the film;
2) And (3) sticking: mixing a hardener with resin to obtain G1 glue, smearing the G1 glue on the surfaces of the cut and treated films, attaching the surfaces of the two films together, and baking and curing;
3) Cutting again: cutting the cured sample into a plurality of thin slices along the normal direction;
4) Mechanical polishing: adhering the cut sample to a sample stage, placing the sample stage on a rotary table, and polishing two sides of the sample in a grading manner; polishing the sample step by adopting different sand paper with the thickness of 500 mu m, and using 200-mesh sand paper with the rotating speed of 800-1000r/min; 1000-mesh sand paper with the thickness of 100 micrometers is used, and the rotating speed is 600-800r/min;
reducing the thickness of the thin film region to below 1 mu m; separating the sample from the sample table to finish mechanical thinning of the transmission electron microscope sample;
5) Ion thinning:
and simultaneously thinning the two sides, controlling the voltage to be 100-500 Kev, and thinning each side for 3-5min, wherein the thickness of the sample is less than 0.1 micrometer, so as to obtain the transmission electron microscope sample of the multilayer film.
2. The method for preparing a transmission electron microscope sample of the multilayer film according to claim 1, wherein the surface is further wiped clean by a cotton swab dipped with acetone under an optical microscope, and finally the acetone on the surface of the film is removed by alcohol.
3. The method for preparing a transmission electron microscope sample of a multilayer film according to claim 1, wherein the hardener is mixed with the resin in the mass ratio of (1-3) (8-12).
4. A method of preparing a transmission electron microscope sample of a multilayer thin film according to claim 3 wherein the hardener is polyamide curing agent 650, 651.
5. The method for preparing a transmission electron microscope sample of a multilayer film according to claim 1, wherein the step of polishing the sample comprises the steps of firstly using 100-mesh diamond sand paper, and replacing diamond particles with 500-1000-mesh sand paper after the surface of the sample is leveled; finally polishing with sand paper of 0.5 mu m or 0.1 mu m, and finishing the first surface polishing after confirming no scratch; and then polishing the second surface, and determining different sand paper and rotating speeds according to different thicknesses.
6. The method for preparing a transmission electron microscope sample of a multilayer film according to claim 1, wherein the sample is cut by a diamond wire cutting machine.
7. A transmission electron microscope sample of the multilayer film prepared by the method of any one of claims 1-6.
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| CN202111343001.2A CN114088751B (en) | 2021-11-12 | 2021-11-12 | Multilayer film transmission electron microscope sample and preparation method thereof |
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| CN202111343001.2A CN114088751B (en) | 2021-11-12 | 2021-11-12 | Multilayer film transmission electron microscope sample and preparation method thereof |
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| CN114088751A CN114088751A (en) | 2022-02-25 |
| CN114088751B true CN114088751B (en) | 2024-04-16 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1068683A (en) * | 1996-08-28 | 1998-03-10 | Kawasaki Steel Corp | Preparation of film specimen for transmission electron microscope |
| CN102023111A (en) * | 2010-11-02 | 2011-04-20 | 大连理工大学 | Method for preparing transmission electron microscope sample of soft brittle phototransistor |
| KR20150090004A (en) * | 2015-07-20 | 2015-08-05 | 국립대학법인 울산과학기술대학교 산학협력단 | Method for producing samples for transmission electron microscopy using tripod polishing and focused ion beam |
| CN105628468A (en) * | 2015-12-28 | 2016-06-01 | 西安电子科技大学 | Method for preparing GaN-based heterojunction transparent film transmission electron microscope sectional sample |
| CN110530691A (en) * | 2019-08-02 | 2019-12-03 | 西安交通大学 | A kind of preparation method of Ultrafine Grained Steel EBSD sample |
| CN113406120A (en) * | 2021-05-24 | 2021-09-17 | 华南理工大学 | Preparation method of metal friction layer transmission electron microscope sample |
-
2021
- 2021-11-12 CN CN202111343001.2A patent/CN114088751B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1068683A (en) * | 1996-08-28 | 1998-03-10 | Kawasaki Steel Corp | Preparation of film specimen for transmission electron microscope |
| CN102023111A (en) * | 2010-11-02 | 2011-04-20 | 大连理工大学 | Method for preparing transmission electron microscope sample of soft brittle phototransistor |
| KR20150090004A (en) * | 2015-07-20 | 2015-08-05 | 국립대학법인 울산과학기술대학교 산학협력단 | Method for producing samples for transmission electron microscopy using tripod polishing and focused ion beam |
| CN105628468A (en) * | 2015-12-28 | 2016-06-01 | 西安电子科技大学 | Method for preparing GaN-based heterojunction transparent film transmission electron microscope sectional sample |
| CN110530691A (en) * | 2019-08-02 | 2019-12-03 | 西安交通大学 | A kind of preparation method of Ultrafine Grained Steel EBSD sample |
| CN113406120A (en) * | 2021-05-24 | 2021-09-17 | 华南理工大学 | Preparation method of metal friction layer transmission electron microscope sample |
Non-Patent Citations (1)
| Title |
|---|
| Growth of Gold Nanoplates: The Case of a Self-Repair Mechanism;Shengchun Yang等;《CRYSTAL GROWTH & DESIGN》;第第7卷卷(第第11期期);第2258-2261页 * |
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