CN114368753A - Reconstructed ternary layered ceramic VSnC crystal and electron beam irradiation treatment method thereof - Google Patents
Reconstructed ternary layered ceramic VSnC crystal and electron beam irradiation treatment method thereof Download PDFInfo
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Abstract
The invention discloses a reconstructed ternary layered ceramic VSnC crystal and an electron beam irradiation treatment method thereof, which comprises the following steps of preparing ternary layered ceramic VSnC powder; step two, preparing a transmission electron microscope sample, placing the transmission electron microscope sample in a transmission electron microscope, and searching a region which is flat in surface, uniform in thickness, free of pollution and parallel to the irradiation direction of the electron beam in the powder sample as an irradiation region; and step three, inducing the material to generate crystal reconstruction. According to the technical scheme, the three-element layered ceramic VSnC crystal is obtained by reasonably proportioning powder materials for preparing the three-element layered ceramic VSnC crystal and optimally designing irradiation parameters, the three-element layered ceramic VSnC crystal is subjected to electron beam irradiation to induce the three-element layered ceramic VSnC crystal to be reconstructed by adopting a conventional electron microscope, and the change of the ceramic VSnC powder microstructure is observed by adopting a projection electron microscope.
Description
Technical Field
The invention relates to the technical field of crystal reconstruction, in particular to a reconstructed ternary layered ceramic VSnC crystal and an electron beam irradiation treatment method thereof.
Background
The lamellar processable MAX phase is a large class of ternary compounds, formula Mn+1AXn, where M is an early transition metal, A is an element from columns 12-16 of the periodic Table of elements, X is carbon, nitrogen or boron, n is an integer, and n can be 1, 2, 3 … …. Depending on the value of n, these compounds are also referred to as 211, 312, 413, etc., the crystal structure of the MAX phase can be regarded as a transition metal carbide, nitride or boride octahedral layer Mn+1XnAnd a layer of a group A element, the majority of the crystal space group being P63/mmc due to its unique nano-layered crystal structure and anisotropic bondingThe properties and the alternative use of metal and ceramic layers in the MAX phase, the chemical bonds of which have the property of mixing covalent ionic metals, show a unique combination of ceramic-like and metal-like properties, and have wide application value. For example, MAX phases are as easy to process as metals, are resistant to thermal shock, are thermally conductive, are electrically conductive, and are resistant to damage; and the ceramic material has the characteristics of low density, high strength and modulus, good corrosion resistance, high temperature oxidation resistance and the like as ceramic. MAX phases are as easy to process as metals, resistant to thermal shock, thermally conductive, electrically conductive, and resistant to damage. And the ceramic material has the characteristics of low density, high strength and modulus, good corrosion resistance, high temperature oxidation resistance and the like as ceramic.
Less research on VSnC systems in MAX phase, V2The SnC crystal structure is mainly crystallized in a hexagonal symmetry mode, the space group is P63/mmc, however, a VSnC system also has a plurality of complex structures, the synthesis interval of the VSnC crystal of the ternary layered ceramic on a phase diagram is narrow, the prepared single-phase substance is difficult to control material sintering, and the influence of the powder property and the biscuit density of the material on densification is serious.
Disclosure of Invention
The invention provides a reconstructed ternary layered ceramic VSnC crystal and an electron beam irradiation treatment method thereof, wherein the reconstructed ternary layered ceramic VSnC crystal is prepared by an electron beam irradiation method, single-phase ternary layered ceramic VSnC crystal is obtained by reasonably proportioning powder materials for preparing the ternary layered ceramic VSnC crystal and optimally designing irradiation parameters, and the technical problems that sintering is difficult, the material powder properties and biscuit density seriously influence densification and the like in the preparation process in the prior art are solved.
The invention is realized by the following technical scheme:
an electron beam irradiation treatment method for reconstructing a ternary layered ceramic VSnC crystal comprises the following steps:
step one, preparing ternary layered ceramic VSnC powder;
preparing a transmission electron microscope sample, placing the transmission electron microscope sample in a transmission electron microscope, and determining a region which is flat in surface, same in thickness and parallel to the irradiation direction of the electron beam in the powder sample as an irradiation region;
and step three, inducing the material to generate crystal reconstruction.
And in the second step, the determined irradiation area is an area with a flat surface, uniform thickness and a crystal band axis parallel to the irradiation direction of the electron beam in the powder sample.
Optionally, in the first step, the method for preparing the ternary layered ceramic VSnC powder comprises: the V powder, the Sn powder and the graphite powder are mixed according to a molar ratio of 2: 1.1: 1, the material is prepared by adopting a pressureless sintering technology.
Alternatively, in a pressureless sintering technique for preparing the ternary layered ceramic VSnC powder, the sintering temperature is 1100 ℃, the ternary layered ceramic VSnC powder is soaked in hydrochloric acid for 10 hours at 60 ℃, and then filtered and cleaned by plasma water and absolute ethyl alcohol.
Optionally, inducing the material to undergo crystal reconstruction in step three is specifically operated as: in a transmission electron microscope, the irradiation voltage of an electron beam is set to be 220kV, and the irradiation time is set to be 5-15 min. Wherein the material is a VSnC powder material.
Optionally, in the third step, the electron beam irradiation induces the crystal reconstruction, the initial phase of the irradiation object is a hexagonal phase, and the reconstruction process is the transformation from the hexagonal phase to the face-centered cubic phase.
Optionally, in the first step, the prepared ternary layered ceramic VSnC powder is trigonal, and the space group is Rm (166).
Optionally, in the third step, in the process of reconstructing the sample by electron beam irradiation treatment, the process of gradually evolving the crystal structure is observed and recorded through a projection electron microscope.
The technical scheme is that a ternary layered ceramic VSnC crystal is obtained by the electron irradiation preparation method, and the experimental formula of the ternary layered ceramic VSnC crystal is V15Sn3C6。
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the technical scheme, the ternary layered ceramic VSnC crystal is subjected to electron beam irradiation induced ternary layered ceramic VSnC crystal reconstruction by adopting a conventional electron microscope, and the change of the ceramic VSnC powder microstructure is observed by a projection electron microscope, so that the whole operation is simple, and the popularization and application values are realized.
2. In the technical scheme, an electron irradiation treatment method is adopted, the VSnC crystal is gradually reconstructed by setting the irradiation voltage and the irradiation time of an electron beam, the heat effect plays a leading role when the irradiation voltage is too low, solid-solid phase change is difficult to realize, the electron carrying energy is too large when the irradiation voltage is too high, a sample wafer is easy to damage, and the setting of the irradiation voltage and the irradiation time is favorable for inducing a sample to generate better crystal reconstruction.
3. According to the technical scheme, crystal reconstruction processing is achieved through a projection electron microscope, the structure evolution process of the VSnC powder can be recorded in real time, and the processing method in the whole experiment process is reliable.
Drawings
FIG. 1 is a schematic block flow diagram of the present invention;
FIG. 2 is a topography of a ternary layered ceramic VSnC crystal and a selected area electron diffraction pattern corresponding thereto;
FIG. 3 is a high resolution chart of the VSnC crystal of the ternary layered ceramic obtained in example 1 irradiated for 5min under 200kV irradiation voltage and a corresponding selected area electron diffraction pattern;
FIG. 4 is a high resolution chart of the VSnC crystal of the ternary layered ceramic obtained in example 1 irradiated for 10min under 200kV irradiation voltage and a selected area electron diffraction pattern corresponding to the high resolution chart;
FIG. 5 is a high resolution diagram of the VSnC crystal of the ternary layered ceramic obtained in example 1 irradiated for 15min under 200kV irradiation voltage and a selected area electron diffraction diagram corresponding to the high resolution diagram.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1:
as shown in fig. 1, an electron beam irradiation treatment method for reconstructing a ternary layered ceramic VSnC crystal comprises the following steps,
step 1: mixing V powder, Sn powder and graphite powder according to a molar ratio of 2: 1.1: 1, synthesizing ternary layered ceramic VSnC powder by adopting a pressureless sintering technology, wherein the sintering temperature is 1100 ℃, the ternary layered ceramic VSnC powder is soaked in hydrochloric acid for 10 hours at the temperature of 60 ℃, and then is filtered and cleaned by using plasma water and absolute ethyl alcohol;
step 2: preparing a transmission electron microscope sample, placing the transmission electron microscope sample in a projection electron microscope, and searching a region which is flat in surface, uniform in thickness, free of pollution and parallel to the irradiation direction of an electron beam in a powder sample as an irradiation region, wherein the irradiation region is shown in figure 1;
and step 3: setting the radiation voltage to be 200kv and the irradiation time to be 5min, and gradually inducing the VSnC crystal of the ternary layered ceramic to be gradually reconstructed.
In the process of inducing the gradual reconstruction of the three-element layered ceramic VSnC crystal, in-situ observation and recording of the crystal reconstruction evolution process of the material are carried out, as shown in figures 3-5, the atomic image of the three-element layered ceramic VSnC crystal irradiation money and a corresponding diffraction pattern are shown, the irradiation area has an obvious crystal structure, and the diffraction pattern is also shown as a trigonal system diffraction pattern. With the irradiation, the sharp spots in the diffraction pattern also gradually change, corresponding to the gradual reconstruction of the hexagonal phase region in the atomic image, and a transition structure in the reconstruction process appears in fig. 4. FIG. 5 is the recorded result after 15 minutes of irradiation, the contrast of the crystal in the atomic image is uniform, and the diffraction pattern is a face centered cubic diffraction pattern, which shows that the three-element layered ceramic VSnC crystal is completely reconstructed into a face centered cubic phase.
Example 2:
the difference from example 1 is that: in the step 3, the radiation voltage is set to be 200kv, and the irradiation time is 10 min.
VSnC ternary layered ceramics prepared in examples 1 and 2 have an empirical formula V15Sn3C6。
Figure 2 is a topographical image and a selected area electron diffraction pattern of a ternary layered ceramic VSnC crystal, which crystallizes in a layered fashion, as other known MAX phases.
FIG. 2(a) shows a selected electron diffraction pattern obtained for the new phase along the [0001] crystallographic band axis.
Fig. 2(b) and 2(d) show selected area electron diffraction patterns of the new phase along different tape axis directions. In the hexagonal system, the extinction law of the diffraction pattern was taken into consideration, and the selective diffraction pattern of the [ hki0] band axis was photographed as shown in FIG. 2 (c).
When the sample was inclined at 30 ° from the domain axis direction of the diffraction pattern in fig. 2(b), the diffraction pattern shown in fig. 2(d) was obtained. The three-element layered ceramic VSnC crystal is known to be a trigonal system with a space group of
FIG. 3 is a high resolution diagram of a ternary layered ceramic VSnC crystal irradiated for 5min under 200kV irradiation voltage and a selected area electron diffraction diagram corresponding to the high resolution diagram. The high resolution graph of FIG. 2 has a center of gravity as an irradiation region, a diffraction pattern with a large number of sharp and regular diffraction spots, and atomic image crystals with band axes of hexagonal phase crystals
FIG. 4 is a high resolution diagram of a ternary layered ceramic VSnC crystal irradiated for 10min under an irradiation voltage of 200kV and a selected area electron diffraction diagram corresponding to the high resolution diagram. A metastable process of hexagonal phase to cubic phase.
FIG. 5 is a high resolution diagram of a ternary layered ceramic VSnC crystal irradiated for 15min under an irradiation voltage of 200kV and a selected area electron diffraction diagram corresponding to the high resolution diagram. Analysis showed that the grains had changed to a face centered cubic phase structure with a crystal orientation of [011 ].
The above-mentioned embodiments, which further illustrate the objects, technical solutions and advantages of the present invention, should be understood that the above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. An electron beam irradiation treatment method for reconstructing a ternary layered ceramic VSnC crystal is characterized by comprising the following steps,
step one, preparing ternary layered ceramic VSnC powder;
preparing a transmission electron microscope sample, placing the transmission electron microscope sample in a transmission electron microscope, and determining a region which is flat in surface, same in thickness and parallel to the irradiation direction of the electron beam in the powder sample as an irradiation region;
and step three, inducing the material to generate crystal reconstruction.
2. The electron beam irradiation treatment method for reconstructing the ternary layered ceramic VSnC crystal according to claim 1, wherein in the first step, the method for preparing the ternary layered ceramic VSnC powder comprises: the V powder, the Sn powder and the graphite powder are mixed according to a molar ratio of 2: 1.1: 1, the material is prepared by adopting a pressureless sintering technology.
3. The electron beam irradiation treatment method for reconstructing the VSnC crystal of the ternary layered ceramic as claimed in claim 2, wherein the sintering temperature of the pressureless sintering technology for preparing the VSnC powder of the ternary layered ceramic is 1100 ℃, the VSnC powder of the ternary layered ceramic is soaked in hydrochloric acid for 10h at 60 ℃, and then filtered and cleaned by plasma water and absolute ethyl alcohol.
4. The electron beam irradiation treatment method for reconstructing the ternary layered ceramic VSnC crystal as claimed in claim 1, wherein the specific operation of inducing the crystal reconstruction of the material in the third step is as follows: in a transmission electron microscope, the irradiation voltage of an electron beam is set to be 220kV, and the irradiation time is set to be 5-15 min.
5. The electron beam irradiation processing method for reconstructing the three-element layered ceramic VSnC crystal as claimed in claim 4, wherein in the third step, the electron beam irradiation induces the crystal reconstruction, the initial phase of the irradiation object is hexagonal phase, and the reconstruction process is the transformation from hexagonal phase to face-centered cubic phase.
6. A reconstructed triplet according to claim 1The electron beam irradiation treatment method of the layered ceramic VSnC crystal is characterized in that in the step one, the prepared ternary layered ceramic VSnC powder is of a trigonal system, and the space group is
7. The electron beam irradiation treatment method for reconstructing the VSnC crystal of the ternary layered ceramic according to claim 6, wherein in the second step, the thickness of the VSnC crystal of the projection electron microscope sample is less than 100nm, and the tape axis is the same as the tape axis
Parallel to the electron beam irradiation direction.
8. The electron beam irradiation processing method for reconstructing the three-element layered ceramic VSnC crystal according to claim 7, wherein in the third step, the process of gradually evolving the crystal structure is observed and recorded by a projection electron microscope during the reconstruction of the electron beam irradiation processed sample.
9. A ternary layered ceramic VSnC crystal obtained by the process according to any of claims 1 to 8, characterized in that it has an empirical formula V15Sn3C6。
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| US20160030913A1 (en) * | 2013-02-13 | 2016-02-04 | Buhei Kono | Method of irradiating a magnetic fluid containing a semiconductor pigment and metal microparticles with microwaves, thereby creatingmixed-phase fluid, and amplifying the superfluid state energy by means of the quantum turbulence phenomenon. |
| WO2016202892A1 (en) * | 2015-06-15 | 2016-12-22 | Katholieke Universiteit Leuven | Max phase ceramics and methods for producing the same |
| US20210122898A1 (en) * | 2018-01-20 | 2021-04-29 | Smart Material Printing, B.V. | Mechanochemical process for producing valuable products free from persistent organic pollutants and other organohalogen compounds from waste comprising plastics and plastic laminates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20160030913A1 (en) * | 2013-02-13 | 2016-02-04 | Buhei Kono | Method of irradiating a magnetic fluid containing a semiconductor pigment and metal microparticles with microwaves, thereby creatingmixed-phase fluid, and amplifying the superfluid state energy by means of the quantum turbulence phenomenon. |
| WO2016202892A1 (en) * | 2015-06-15 | 2016-12-22 | Katholieke Universiteit Leuven | Max phase ceramics and methods for producing the same |
| US20210122898A1 (en) * | 2018-01-20 | 2021-04-29 | Smart Material Printing, B.V. | Mechanochemical process for producing valuable products free from persistent organic pollutants and other organohalogen compounds from waste comprising plastics and plastic laminates |
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