CN115872747B - Scandium-containing ternary layered carbide ceramic material and preparation method and application thereof - Google Patents
Scandium-containing ternary layered carbide ceramic material and preparation method and application thereof Download PDFInfo
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- CN115872747B CN115872747B CN202211461826.9A CN202211461826A CN115872747B CN 115872747 B CN115872747 B CN 115872747B CN 202211461826 A CN202211461826 A CN 202211461826A CN 115872747 B CN115872747 B CN 115872747B
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- 229910052706 scandium Inorganic materials 0.000 title claims abstract description 50
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 230000005855 radiation Effects 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 125000004429 atom Chemical group 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 34
- 239000011812 mixed powder Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005251 gamma ray Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003326 scandium compounds Chemical class 0.000 description 2
- -1 scandium halides Chemical class 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 230000005461 Bremsstrahlung Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000004215 lattice model Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Abstract
The invention discloses a scandium-containing ternary lamellar carbide ceramic material, a preparation method and application thereof, wherein the scandium-containing ternary lamellar carbide ceramic material comprises three elements of scandium, lead and carbon, and the chemical formula is Sc 2 PbC；Sc 2 PbC has a space group of P6 3 And/mmc having a lattice parameter of
Description
Technical Field
The invention relates to the field of materials, in particular to a scandium-containing ternary layered carbide ceramic material, and a preparation method and application thereof.
Background
Scandium (Sc) is a typical rare earth element with an average abundance of 36ppm in the crust and a global scandium reserve of about 200 ten thousand tons, with our scandium resource reserve of about 65 ten thousand tons accounting for 1/3 of the global resource. Based on such a large reserves, our country has natural advantages for the development of sophisticated applications of scandium-containing compounds.
Scandium currently exists in three main forms, simple substance, oxide and halide, respectively. Scandium in the simple substance form is usually used as an additive, and the addition of a trace amount of scandium can greatly optimize the mechanical properties of the aluminum alloy, so that the scandium is one of the most main applications at present; the scandium oxide has wider research compared with simple substance form, can be applied to the directions of alloy, catalysis, laser and the like, and has good application prospect; scandium halides are less useful than the other two, mainly focused on scandium-sodium metal halide lamps. In addition to these three main forms of application, other applications for scandium are continually being explored. Scandium has a good resistance to neutron radiation and can absorb neutrons to form an isotope 46Sc in a nuclear reactor, but the application of scandium is very limited in radiation protection.
Therefore, the application of the scandium expansion element has important significance for the field of materials.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a scandium-containing ternary layered carbide ceramic material, a preparation method and application thereof, and application of scandium element expansion.
The invention is realized by the following technical scheme:
scandium-containing ternary lamellar carbide ceramic material with chemical formula of Sc2PbC, space group of P63/mmc and lattice parameter ofSc atoms are located at (1/3, 2/3,0.57958), pb atoms are located at (1/3, 2/3, 1/4), and C atoms are located at (0, 0).
The preparation method of the scandium-containing ternary layered carbide ceramic material comprises the following steps:
(1) Mixing: stirring and mixing Sc powder, pb powder and C powder to obtain mixed powder;
(2) Sintering: sintering the mixed powder obtained in the step (1);
(3) And (3) cooling: and (3) cooling the mixed powder sintered in the step (2) to room temperature, and grinding off a surface carbonization layer to obtain the scandium-containing ternary layered carbide ceramic material.
Further, in the step (1), the particle size of the Sc powder is 150-250 meshes, the particle size of the Pb powder is 500-800 meshes, and the particle size of the C powder is 300-1500 meshes.
Further, in the step (1), the molar ratio of Sc powder, pb powder and C powder is 2: (0.9-1.3): 1, mixing under the protection of inert gas, preferably argon.
The beneficial effects of adopting further technical scheme are:
the particle size and the proportion of the Sc powder, the Pb powder and the C powder are selected above, which is favorable for forming the Sc finally 2 The microstructure of PbC is mixed under the protection of inert gas, so that air can be discharged, and the phenomenon of oxidation of raw materials is avoided.
Further, the mixing time in the step (1) is 10 to 14 hours, preferably 12 hours, and the mixing speed is 40 to 80rpm, preferably 70rpm.
The beneficial effects of adopting the further technical scheme are as follows:
the further technical scheme can lead the powder to be uniformly mixed, and lead the texture of the sintered ceramic material to be uniform.
Further, in the step (2), after the temperature is raised to 650-750 ℃ at a temperature raising rate of 40-70 ℃/s, the temperature is raised to 1100-1300 ℃ at a temperature raising rate of 10-20 ℃/s, the temperature is kept for 0-60 min, preferably, after the temperature is raised to 700 ℃ at a temperature raising rate of 50 ℃/s, the temperature is raised to 1200 ℃ at a temperature raising rate of 10 ℃/s, and the temperature is kept for 50min.
The beneficial effects of adopting the further technical scheme are as follows:
the first stage is heated, with the rise of temperature, the diffusion of atoms is aggravated, the pores are reduced, the point contact between the powder bodies is changed into the surface contact, the pores between the powder bodies are reduced, and the communicated pores become closed and are distributed in an isolated manner; the second stage of heating causes the small particles to first generate crystal boundary, substances on the crystal boundary are continuously diffused to the pore, the pore is gradually eliminated, the crystal boundary moves, and crystal grains grow up.
Further, the sintering pressure in the step (2) is 20 to 40MPa, preferably 20MPa.
The beneficial effects of adopting the further technical scheme are as follows:
the sintering pressure of 20-40 MPa is used for promoting the grain orientation and densification process under the high temperature effect to form Sc 2 Crystal structure of PbC.
The scandium-containing ternary layered carbide ceramic material is applied to radiation protection.
By adopting the technical scheme, the invention has the beneficial effects that:
the method introduces lead elements with the capability of resisting alpha rays, gamma rays and X rays, and the lead elements can isolate rays and slow down the speed of fast neutrons, and the fast neutrons slowed down by lead are absorbed by scandium elements; carbon elements with lower atomic numbers are introduced, so that the bremsstrahlung of beta rays can be resisted. The scandium-containing ternary layered carbide ceramic material prepared by the method has a shell-shaped layered structure, has good radiation protection performance, is easy to obtain raw materials, is easy to operate, has simple equipment, provides a brand new idea for designing the comprehensive radiation protection material, and widens the application range of scandium elements.
Drawings
FIG. 1 shows a ternary layered scandium-containing compound Sc 2 X-ray diffraction patterns (a) and Sc of PbC ceramic material 2 A comparison of the theoretical X-ray diffraction pattern (b) of PbC ceramic material.
FIG. 2 shows a ternary layered scandium-containing compound Sc 2 A micro-topography map (a) and an X-ray energy chromatogram (b) of the PbC ceramic material.
FIG. 3 shows a ternary layered scandium compound Sc 2 Atomic arrangement pattern (b) and theoretical diffraction spot diagram (c) of the (a), (0002) plane and atomic arrangement pattern (d) and theoretical diffraction spot diagram (e) of the (1120) plane of the PbC ceramic material.
FIG. 4 shows a ternary layered scandium compound Sc 2 Rietveld fit of PbC ceramic material.
Detailed Description
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
A preparation method of scandium-containing ternary layered carbide ceramic material comprises the following steps:
(1) Sc powder (99.9%, 200 mesh), pb powder (99.99%, 500 mesh) and carbon powder (99.95%, 500 mesh) were mixed in a molar ratio of 2:1:1, mixing, namely mixing materials for 12 hours by using a drum mixer under the protection of argon gas to obtain mixed powder;
(2) 15g of mixed powder is put into a graphite mould filled with graphite paper, a graphite felt is sleeved, the mixed powder is loaded into a discharge plasma furnace, the temperature is increased to 700 ℃ at a heating rate of 50 ℃/min under 20MPa, then the mixed powder is heated to 1200 ℃ at a heating rate of 10 ℃/min, and the mixed powder is cooled along with the furnace after heat preservation for 50 min; and grinding the surface carbide layer to obtain the target block.
Example 2
A preparation method of scandium-containing ternary layered carbide ceramic material comprises the following steps:
(1) Sc powder (99.9%, 200 mesh), pb powder (99.99%, 500 mesh) and carbon powder (99.95%, 300 mesh) in a molar ratio of 2:1.1:1, mixing, namely mixing materials for 14 hours by using a drum mixer under the protection of argon gas to obtain mixed powder;
(2) 15g of mixed powder is put into a graphite mould filled with graphite paper, a graphite felt is sleeved, the mixed powder is loaded into a discharge plasma furnace, the temperature is raised to 700 ℃ at a heating rate of 40 ℃/s under 20MPa, then the temperature is raised to 1100 ℃ at 20 ℃/min, and the mixed powder is cooled along with the furnace after heat preservation for 20 min; and grinding the surface carbide layer to obtain the target block.
Example 3
A preparation method of scandium-containing ternary layered carbide ceramic material comprises the following steps:
(1) Sc powder (99.9%, 200 mesh), pb powder (99.99%, 800 mesh) and carbon powder (99.95%, 1500 mesh) in a molar ratio of 2:0.9:1, mixing, namely mixing materials for 10 hours by using a drum mixer under the protection of argon gas to obtain mixed powder;
(2) 15g of mixed powder is put into a graphite mould filled with graphite paper, a graphite felt is sleeved, the mixed powder is loaded into a discharge plasma furnace, the temperature is increased to 700 ℃ at the temperature increasing rate of 70 ℃/s under 20MPa, then the temperature is increased to 1300 ℃ at 15 ℃/min, and the mixed powder is cooled along with the furnace; and grinding the surface carbide layer to obtain the target block.
Experimental example 1
(1) Sc obtained in example 1 2 The PbC ceramic Material blocks were phase-detected using X-ray diffraction (XRD) and characteristic peaks of the new phase were identified corresponding to the theoretical characteristic peaks calculated by the Material Studio, as shown in FIG. 1.
Sc prepared in example 1 according to the X-ray diffraction pattern (a) of the ceramic material powder shown in FIG. 1 2 The PbC ceramic material block X-ray diffraction has a series of unknown peaks, and the peak positions of the unknown peaks are equal to Sc 2 The theoretical X-ray diffraction pattern (b) of PbC is highly consistent.
(2) Sc obtained in example 1 2 The PbC ceramic material blocks were observed for microscopic morphology using a scanning electron microscope in combination with an energy spectrometer (SEM/EDS), as shown in FIG. 2.
According to the micro-morphology of the ceramic powder shown in FIG. 2, powder Sc prepared in example 1 2 PbC has typical lamellar features and the white cross-position X-ray energy chromatogram (b) results show Sc: pb=2: 0.95, within the tolerance limits.
(3) Identifying the XRD pattern obtained in step (1), and calculating Sc by using Crystal Maker in combination with the theoretical Crystal structure calculated by Material Studio 2 The diffraction spots of the PbC theory are shown in FIG. 3.
Sc established according to example 1 shown in FIG. 3 2 A lattice (a) of PbC ceramic material, wherein both the atomic arrangement pattern (b) and the theoretical diffraction pattern (c) of the (0002) plane show that it belongs to the hexagonal system,the atomic arrangement pattern (d) and the theoretical diffraction spot pattern (e) of the face show typical lamellar arrangements, sc and Pb atomic boundaries [0001 ]]Direction is ABABABIn a regular stack.
(4) Taking the XRD pattern obtained in the step (1) and the optimized lattice model as inputs, and performing Rietveld fitting in Full-Prof software to obtain Sc 2 PbC ceramic materialRietveld fit of the material is shown in fig. 4. The lattice constants, atomic positions of the ceramic material powders are determined as shown in table 1, and the 2θ, d, I values of the different crystal planes are calculated and tested as shown in table 2.
TABLE 1Sc 2 Lattice constant and atomic position of PbC ceramic material
TABLE 2 calculation and experiment of 2 theta, d and I values corresponding to different crystal planes of ceramic material
According to FIG. 4, sc 2 Rietveld fitted plot of PbC ceramic material blocks, representing Difference, scC, sc in sequence from bottom to top 3 Pbc, and Sc 2 PbC, the uppermost layer is that Raw data overlaps with calcualted line, sc 2 The purity of the PbC sample was 87.40wt% (11.69 wt% Sc contained therein) 3 PbC,0.91wt% scc), the error value was R-p=13.90% and R-wp=18.40%.
Experimental example 1
The scandium-containing ternary layered carbide ceramic materials prepared in examples 1 to 4 were subjected to gamma ray and neutron ray shielding performance tests, and simulation tests were performed by using a Monte Carlo MCNP program, and the results are shown in Table 3.
TABLE 3 performance of scandium-containing ternary layered carbide ceramic materials in shielding gamma rays and neutron rays
From the data in Table 3, the scandium-containing ternary layered carbide ceramic material prepared by the invention has good shielding performance and stronger gamma ray and neutron ray absorption capability.
The invention relates to a scandium-containing ternary layered carbide ceramic material Sc 2 PbC and preparation method thereof, and the method of the invention is adopted to successfully prepare new Sc 2 PbC ceramic material with better radiation protection capability and Sc 2 The lattice structure parameter and the X-ray diffraction data of PbC provide a brand new idea of designing the comprehensive radiation-proof material, and widen the application range of scandium element.
Claims (6)
1. A scandium-containing ternary lamellar carbide ceramic material is characterized in that the chemical formula of the scandium-containing ternary lamellar carbide ceramic material is Sc 2 PbC, space group P6 3 /mmc, lattice parameter ofSc atoms are located at (1/3, 2/3,0.57958), pb atoms are located at (1/3, 2/3, 1/4), and C atoms are located at (0, 0);
the preparation method comprises the following steps:
(1) Mixing: ball milling and mixing Sc powder, pb powder and C powder to obtain mixed powder;
(2) Sintering: sintering the mixed powder obtained in the step (1); the sintering process is as follows: heating to 650-750 ℃ at a heating rate of 40-70 ℃/s, heating to 1100-1300 ℃ at a heating rate of 10-20 ℃/s, and preserving heat for 0-60 min; the sintering pressure is 20-40 MPa;
(3) And (3) cooling: and (3) cooling the mixed powder sintered in the step (2) to room temperature, and grinding off a surface carbonization layer to obtain the scandium-containing ternary layered carbide ceramic material.
2. The scandium-containing ternary layered carbide ceramic material according to claim 1, wherein in step (1), the particle size of Sc powder is 150 to 250 mesh, the particle size of Pb powder is 500 to 800 mesh, and the particle size of C powder is 300 to 1500 mesh.
3. The scandium-containing ternary layered carbide ceramic material according to claim 1, wherein the molar ratio of Sc powder, pb powder and C powder in step (1) is 2: (0.9-1.3): 1, mixing under the protection of inert gas.
4. The scandium-containing ternary layered carbide ceramic material according to claim 1, wherein the mixing time in step (1) is 10-14 h and the mixing speed is 40-80 rpm.
5. The scandium-containing ternary layered carbide ceramic material according to claim 4, wherein the mixing time in step (1) is 12h and the mixing speed is 70rpm.
6. The use of a scandium-containing ternary layered carbide ceramic material according to claim 1 for protection against radiation.
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| US20210101839A1 (en) * | 2018-06-20 | 2021-04-08 | Drexel University | Ceramic oxide composites reinforced with 2d mx-enes |
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