CN113816378B - MAX phase layered material containing antimony element at A position, preparation method and application thereof - Google Patents
MAX phase layered material containing antimony element at A position, preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 120
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 27
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 150000003624 transition metals Chemical group 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 42
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 150000003839 salts Chemical class 0.000 claims description 10
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 8
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 5
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 229910018989 CoSb Inorganic materials 0.000 claims description 2
- 241000080590 Niso Species 0.000 claims description 2
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- -1 naBr Chemical compound 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 238000004146 energy storage Methods 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- QDNXSIYWHYGMCD-UHFFFAOYSA-N 2-(methylamino)-1-(3-methylphenyl)propan-1-one Chemical compound CNC(C)C(=O)C1=CC=CC(C)=C1 QDNXSIYWHYGMCD-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 20
- 239000008367 deionised water Substances 0.000 description 18
- 229910021641 deionized water Inorganic materials 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910006913 SnSb Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 230000001276 controlling effect Effects 0.000 description 2
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- 239000006228 supernatant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910016345 CuSb Inorganic materials 0.000 description 1
- 229910020037 NbSb Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/0828—Carbonitrides or oxycarbonitrides of metals, boron or silicon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention discloses an A-site antimony-containing MAX phase layered material, a preparation method and application thereof. The MAX phase lamellar material is a nano lamellar compound with a molecular formula of M n+ 1 AX n M is selected from any one or any combination of more than two of the pre-transition metal group elements, A is any combination of antimony or antimony-containing alloy, X is C and/or N element, and N is 1,2, 3 or 4. The A-site MAX phase layered material containing antimony element provided by the invention has a hexagonal crystal system structure, and the space group is P6 3 Mmc, unit cell is composed of M n+1 X n The substructure layer and the atomic layer containing antimony are alternately stacked. The MAX phase layered material containing the A-site antimony element provided by the invention has potential application prospects in the fields of superconduction, energy storage, catalysis, electromagnetic shielding, friction and abrasion and the like.
Description
Technical Field
The invention relates to an inorganic material, in particular to a novel MAX phase layered material containing an A-site antimony element, and a preparation method and application thereof, and belongs to the technical field of materials.
Background
M n+1 AX n The phase material is a ternary layer nano lamellar compound, M-site element is usually a front transition group metal element, A-site element is mainly III A group and IV A group element, X-site element is C and/or N, wherein n=1, 2 or 3. The crystal structure of MAX phase is hexagonal crystal structure, and the space group is P6 3 Mmc, made of M n+1 X n The nanometer sublayer structure and the A atomic layer are alternately stacked, wherein M n+1 X n Co-edge M of nanostructure sublayer by covalent bond 6 The X octahedron layer is composed, the adjacent MX sublayer structures are in twin phase, and X is positioned in an octahedral gap formed by M atoms. Theoretical calculation prediction shows that more than 600 MAX phases have thermodynamic stability, wherein the number of the pure MAX phases which are successfully synthesized is more than 70. The M-bit, A-bit and X-bit element distributions of the MAX phase have been found to include 25M-bit elements, 18A-bit elements (Al, si, P, S, ga, ge, as, in, sn, tl, pb, bi, cu, zn, pd, ir, au, cd) and 2X-bit elements. The MAX phase has rich chemical element composition, so that the physical and chemical properties of the MAX phase can be changed and regulated by regulating the element types and the relative contents of the MAX phase, and meanwhile, the diversity of MAX phase materials can be greatly enriched. However, preparation of MAX phase with the A-bit being Sb element is not successfully realized at present.
Disclosure of Invention
The invention mainly aims to provide an A-site MAX phase layered material containing antimony element and a preparation method thereof, thereby overcoming the defects in the prior art.
The invention also aims at providing application of the MAX phase layered material containing the A-site antimony element.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides an A-site MAX phase layered material containing antimony element, wherein the molecular formula of the MAX phase layered material is expressed as M n+1 AX n Wherein M is selected from any one or any combination of more than two of the elements in the front transition metal group, A is any combination of antimony or antimony-containing alloy, X is C, N elementAny one or any combination of two of the above, n is 1,2, 3 or 4.
In some embodiments, a is Sb, or an antimony-containing alloy formed by any one or any combination of two or more of Sb and Al, si, P, S, ga, ge, as, in, sn, tl, pb, bi, fe, co, ni, cu, zn, pd, ir, au, cd, se, te.
The embodiment of the invention also provides a preparation method of the MAX phase layered material containing the antimony element at the A site, which comprises the following steps: m and/or M-containing material, A and/or A-containing material, X and/or X-containing material according to the following weight ratio (2-4): 1: uniformly mixing the components (1-3) according to the molar ratio, and reacting the obtained mixture in an inert atmosphere at a high temperature of 400-1700 ℃ for 30-120 min to obtain the MAX phase layered material containing the antimony element at the A site;
or, precursor MAX phase material, A and/or material containing A, metal fused salt and inorganic salt are mixed according to the proportion of 1: (1-3): (2-3): (3-10), and carrying out high-temperature reaction on the obtained mixture in an inert atmosphere at 400-1700 ℃, and then carrying out post-treatment to obtain the A-site MAX phase layered material containing antimony elements;
wherein the molecular formula of the precursor MAX phase material is expressed as M m+1 A’X m Wherein M is selected from a group III B, IV B, V B or VI B pre-transition metal element, a' is selected from a group iiia or IV a element, X comprises C and/or N, m=1, 2 or 3. Further, the precursor MAX phase material comprises Ti 3 AlC 2 、Ti 2 AlC、Ti 2 AlN、Ti 4 AlN 3 、V 2 AlC、Cr 2 AlC、Nb 2 AlC、Hf 2 AlN、Ta 4 AlC 3 、Ti 3 Any one or a combination of two or more of AlCN, but not limited thereto. Compared with the prior art, the invention has at least the following advantages:
(1) The preparation method of the A-site antimony-containing MAX phase layered material provided by the embodiment of the invention realizes the preparation of the novel MAX phase material with A being the antimony element for the first time, and the preparation method is simple and has universality;
(2) The MAX phase layered material A-site element contains antimony element, has the characteristics of metal and ceramic, and has the characteristics of high strength, high hardness, high heat conduction, high electric conduction, oxidation resistance, high temperature resistance, high damage tolerance, processability and the like. The introduction of the antimony element causes the electronic structure of the material to be greatly changed compared with the existing MAX phase material, so that the physical and chemical properties of the MAX phase material are changed, and the physical and chemical properties of the MAX phase material are regulated and controlled by introducing the antimony element, so that the synthesized novel MAX phase material has potential application prospect in the fields of superconduction, energy storage, catalysis, electromagnetic shielding, friction and abrasion and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. The drawings in the following description are only examples of embodiments of the present invention and other drawings may be obtained from them by those skilled in the art without inventive effort.
FIG. 1 is a MAX phase layered material Nb containing an antimony element at the A-position in example 1 of the present invention 2 SbC XRD pattern;
FIG. 2 is a MAX phase layered material Nb containing antimony element at the A-position in example 1 of the present invention 2 SbC XRD pattern Reitveld method refinement analysis result pattern;
FIG. 3 is a MAX phase layered material Nb containing antimony element at the A-position in example 1 of the present invention 2 SbC spherical aberration correcting high-resolution transmission electron microscope image and atomic-level element distribution image;
FIG. 4 is a MAX phase layered material Ti containing antimony element at A-position in example 2 of the invention 3 SbC 2 An XRD pattern of (b);
FIG. 5 is a MAX phase layered material Ti containing antimony element at A-position in example 2 of the invention 3 SbC 2 Spherical aberration correction high-resolution transmission electron microscope images and atomic-level element distribution diagrams;
FIG. 6 is a MAX phase layered material Ti containing antimony element at A-position in example 3 of the invention 3 XRD pattern of SbCN;
FIG. 7 is a MAX phase layered material Ti containing antimony element at A-position in example 3 of the invention 3 SbCN edgeSpherical aberration correction high-resolution transmission electron microscope and atomic schematic diagram of crystal band axis;
FIG. 8 is a MAX phase layered material Ti containing antimony element at A-position in example 3 of the invention 3 Spherical aberration correction high-resolution transmission electron microscope image and atomic-level element distribution image of SbCN.
Detailed Description
The MAX phase material for synthesizing the A-site antimony-containing element has very important significance for supplementing MAX phase definition, expanding the composition types and regulating and controlling the chemical properties of substances; secondly, by utilizing the diversity and rich adjustability of the A-bit element of the MAX phase material, a brand new MAX phase material containing the A-bit antimony element can be synthesized, and the material synthesis method is an innovation and provides brand new synthesis strategies for synthesis of other novel MAX phases; in addition, the MAX phase material containing the A-site antimony element is synthesized, and the structure and the property of the MAX phase material are regulated and controlled by regulating and controlling the content, the position and the type of the A-site element, so that the purpose of application of the MAX phase material in the fields of superconducting, energy storage and the like is achieved.
Therefore, the technical principle of the inventor is as follows: the antimony element is introduced into the A-site atomic layer of the MAX phase material, so that the electronic structure of the MAX phase material is greatly changed compared with the existing MAX phase material, thereby causing the physical and chemical properties of the MAX phase material to be changed, and the MAX phase material has potential application prospect in the fields of superconducting, energy storage, catalysis, biology, microwave devices and the like.
One aspect of the embodiment of the invention provides a MAX phase lamellar material containing an antimony element at the A position, wherein the molecular formula of the MAX phase lamellar material is represented as M n+1 AX n Wherein M is selected from any one or any combination of more than two of the elements in the front transition metal group, A is any combination of antimony or antimony-containing alloy, X is any one or any combination of two of the elements C, N, and n is 1,2, 3 or 4.
In some embodiments, the M includes any one or a combination of two or more of Sc, ti, V, cr, mn, Y, zr, nb, mo, hf, ta, W and the like, and is not limited thereto.
In some embodiments, a is Sb, or an antimony-containing alloy formed by any one or any combination of two or more of Sb and Al, si, P, S, ga, ge, as, in, sn, tl, pb, bi, fe, co, ni, cu, zn, pd, ir, au, cd, se, te.
In some embodiments, X is C x N y Wherein x+y=1 to 2.
Further, the MAX phase layered material containing antimony element at the A site has a hexagonal crystal system structure, and the space group is P6 3 Mmc, unit cell is composed of M n+1 X n The substructure layer and the atomic layer containing antimony are alternately stacked.
The preparation method of the MAX phase layered material containing the A-site antimony element provided by the other aspect of the embodiment of the invention comprises the following steps: m and/or M-containing material, A and/or A-containing material, X and/or X-containing material according to the following weight ratio (2-4): 1: uniformly mixing the components (1-3) according to the molar ratio, and reacting the obtained mixture in an inert atmosphere at a high temperature of 1000-1700 ℃ for 30-120 min to obtain the A-site MAX phase layered material containing the Sb element;
or, precursor MAX phase material, A and/or material containing A, metal fused salt and inorganic salt are mixed according to the proportion of 1: (1-3): (2-3): (3-10), and carrying out high-temperature reaction for 30-120 min at 400-1000 ℃ in inert atmosphere, and then carrying out post-treatment to obtain the A-site MAX phase layered material containing antimony elements;
wherein the molecular formula of the precursor MAX phase material is expressed as M m+1 A’X m Wherein M is selected from a group III B, IV B, V B or VI B pre-transition metal element, a' is selected from a group iiia or IV a element, X comprises C and/or N, m=1, 2 or 3. The molecular formula of the MAX phase lamellar material prepared by the invention is expressed as M n+1 AX n Wherein M is selected from any one or any combination of more than two of the elements of the front transition metal group, A is any combination of antimony or antimony-containing alloy, X is any one or any combination of two of the elements C, N, and n is 1,2, 3 or 4.
In some embodiments, the precursor MAX phase material comprises Ti 3 AlC 2 、Ti 2 AlC、Ti 2 AlN、Ti 4 AlN 3 、V 2 AlC、Cr 2 AlC、Nb 2 AlC、Hf 2 AlN、Ta 4 AlC 3 、Ti 3 AlCN, etc., but is not limited thereto.
In some embodiments, the molten metal salt includes FeO, fe 2 O 3 、CoO、NiO、CuO、ZnO、CdO、Ag 2 O、FeCl 2 、FeCl 3 、CoCl 2 、NiCl 2 、CuCl 2 、CuCl、ZnCl 2 、CdCl 2 、AgCl、FeBr 2 、FeBr 3 、CoBr 2 、NiBr 2 、CuBr 2 、CuBr、ZnBr 2 、CdBr 2 、AgBr、FeI 2 、CoI 2 、NiI 2 、CuI、ZnI 2 、CdI 2 、AgI、FeSO 4 、Fe 2 (SO 4 ) 3 、CoSO 4 、NiSO 4 、CuSO 4 、Cu 2 SO 4 、ZnSO 4 、CdSO 4 、Ag 2 SO 4 Any one or a combination of two or more of these, etc., but is not limited thereto.
In some embodiments, the M-containing material includes an alloy containing elemental M and/or M, but is not limited thereto.
Further, the a-containing material includes an alloy containing a simple substance and/or a, but is not limited thereto.
Further, the A and/or A-containing materials (Sb and alloys thereof) include Sb, cdSb, ag 2 Sb、CoSb、Cu 2 Sb、FeSb、FeSb 2 Any one or a combination of two or more of NiSb, snSb, znSb, etc., but is not limited thereto.
Further, the inorganic salt includes any one or a combination of two or more of NaF, naK, liCl, naCl, KCl, naBr, KBr and the like, but is not limited thereto.
Another aspect of the embodiment of the invention also provides the use of any of the foregoing MAX-phase layered materials containing an antimony element at the a-site in fields of superconducting, energy storage, and the like.
The present invention will be described in further detail with reference to the following examples, which are intended to facilitate the understanding of the present invention without any limitation thereto.
Example 1: in this embodiment, the MAX phase layered material with the A site being the antimony element is Nb 2 SbC powder material.
The Nb is 2 The preparation method of SbC powder comprises the following steps:
(1) Weighing metal Nb powder (purity of 99.99 wt.%) with 500 meshes and Sb powder (purity of 99.99 wt.%) with 300 meshes in a molar ratio of 2:1:1, and grinding and mixing the materials to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1000 ℃, the heat preservation time is 30min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Crushing, grinding and sieving the reaction product to obtain a powder sample.
The powder treated in step (3) was detected by X-ray diffraction (XRD) (see fig. 1). The full spectrum analysis by the Reitveld method can obtain that the theoretical simulation result is highly consistent with the experimental result (R wp =9.8%), demonstrating that this method successfully synthesizes Nb 2 SbC MAX phase material (fig. 2) has a lattice constant of a=0.3314 nm and c= 1.3239nm. Small amounts of NbSb present in the powder 2 Alloy phase impurities are by-products in this reaction.
FIG. 3 is MAX phase Nb 2 SbC spherical aberration correcting high resolution transmission electron microscope image and atomic level element distribution map. It can be clearly seen that the two alternately stacked nanostructures are made of Nb 2 A C layer and an Sb atomic layer. The atomic position can be clearly distinguished through atomic-level energy spectrum surface scanning analysis and line scanning analysis, and Nb is quantitatively analyzed through energy spectrum, namely, sb is approximately equal to 2:1, and the atomic position is equal to Nb 2 The stoichiometric ratios of the elements in SbC are matched. So the chemical expression of the obtained novel MAX phase material is Nb 2 SbC。
Example 2: in this embodiment, the MAX phase layered material with the A site being the antimony element is Ti 3 SbC 2 A bulk material.
The Ti is 3 SbC 2 The preparation method of the block comprises the following steps:
(1) Weighing metal Ti powder (purity is 99.99 wt.%) with 500 meshes and Sb powder (purity is 99.99 wt.%) with 300 meshes, and graphite powder with 300 meshes, wherein the molar ratio of the metal Ti powder to the graphite powder is 3:1:2, grinding and mixing the materials to obtain a mixture.
(2) And pressing the mixture into a tablet by using a graphite die, and then placing the tablet into a spark plasma sintering system for reaction. The reaction conditions are as follows: the reaction temperature is 1300 ℃, the heat preservation time is 50min, and the inert atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the graphite mold.
(3) Washing the reaction product with deionized water and alcohol: grinding the reaction product to remove the surface graphite layer, putting the reaction product into a beaker, adding deionized water, stirring and ultrasonically cleaning for 30 minutes, standing for 1 hour, and pouring out supernatant. Washing the reaction product for three times, washing with ethanol, putting the reaction product into a baking oven at 40 ℃ and taking out the reaction product after 12 hours to obtain a solid product.
FIG. 4 shows the Ti after the treatment of step (3) 3 SbC 2 XRD patterns of the bulk sample are typical 211 MAX phase XRD pattern characteristic peak types. FIG. 5 is MAX phase Ti 3 SbC 2 Spherical aberration correcting high-resolution transmission electron microscope image and atomic-level element distribution map. It is clear from this that the two alternately stacked nanostructures are made of Ti 3 C 2 A layer and an atomic layer of Sb. The atomic position can be clearly distinguished through atomic level energy spectrum surface scanning analysis and line scanning analysis, and the atomic position is quantitatively analyzed through energy spectrum to be Ti: sb apprxeq 3:1, and the atomic position is compared with Ti 3 SbC 2 The stoichiometric ratios of the elements are identical. So the chemical expression of the obtained novel MAX phase material is Ti 3 SbC 2 。
Example 3: in this embodiment, the MAX phase layered material with the A site being the antimony element is Ti 3 SbCN bulk material.
The Ti is 3 The preparation method of the SbCN block comprises the following steps:
(1) Weighing the molar ratio of 2:1:1:1 (purity 99.99 wt.%), ti powder (purity 99.99 wt.%), 300-mesh Sb powder (purity 99.99 wt.%) and 300-mesh graphite powder, and grinding and mixing the above materials to obtain a mixture.
(2) And pressing the mixture into a tablet by using a graphite die, and then placing the tablet into a spark plasma sintering system for reaction. The reaction conditions are as follows: the reaction temperature is 1700 ℃, the heat preservation time is 30min, and the inert atmosphere is protected. And after the temperature of the sintering system is reduced to room temperature, taking out the reaction product in the graphite mold.
(3) Washing the reaction product with deionized water and alcohol: grinding the reaction product to remove the surface graphite layer, putting the reaction product into a beaker, adding deionized water, stirring and ultrasonically cleaning for 30 minutes, standing for 1 hour, and pouring out supernatant. Washing the reaction product for three times, washing with ethanol, putting the reaction product into a baking oven at 40 ℃ and taking out the reaction product after 12 hours to obtain a solid product.
FIG. 6 shows the Ti after the treatment of step (3) 3 XRD pattern of SbCN bulk sample. FIG. 7 is Ti 3 SbCN edgeSpherical aberration correction high-resolution transmission electron microscope and atomic schematic diagram of crystal band axis. FIG. 8 is MAX phase Ti 3 Spherical aberration correction high-resolution transmission electron microscope image and atomic-level element distribution image of SbCN. It is clear from this that the two alternately stacked nanostructures are made of Ti 3 CN layer and Sb atomic layer. The atomic position can be clearly distinguished through atomic level energy spectrum surface scanning analysis and line scanning analysis, and the atomic position is quantitatively analyzed through energy spectrum to be Ti: sb apprxeq 3:1, and the atomic position is compared with Ti 3 The stoichiometric ratios of the elements in SbCN are identical. So the chemical expression of the obtained novel MAX phase material is Ti 3 SbCN。
Example 4: in this embodiment, the MAX phase layered material with the A site being the antimony element is Ti 3 SbC 2 Powder material.
The Ti is 3 SbC 2 The preparation method of the powder comprises the following steps:
(1) Weighing 500-mesh metal Ti powder (purity 99.99 wt.%) and 300-mesh Sb powder (purity 99.99 wt.%) with a molar ratio of 3:1:2, and grinding and mixing the materials to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1500 ℃, the heat preservation time is 120min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, and after stirring and ultrasonic cleaning for 30 minutes, the remaining salt in the reaction product was washed away, followed by suction filtration. And finally, cleaning the treated reaction product with ethanol, putting the cleaned reaction product into a baking oven at 40 ℃, and taking out the reaction product after 12 hours to obtain a powder product.
Example 5: in this embodiment, the MAX phase layered material with the A site being the antimony element is Nb 4 SbC 3 Powder material.
The Nb is 4 SbC 3 The preparation method of the powder comprises the following steps:
(1) Weighing 500-mesh metal Nb powder (purity of 99.99 wt.%) and 300-mesh Sb powder (purity of 99.99 wt.%) with a molar ratio of 4:1:3, and grinding and mixing the materials to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1400 ℃, the heat preservation time is 120min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, and after stirring and ultrasonic cleaning for 30 minutes, the remaining salt in the reaction product was washed away, followed by suction filtration. And finally, cleaning the treated reaction product with ethanol, putting the cleaned reaction product into a baking oven at 40 ℃, and taking out the reaction product after 12 hours to obtain a powder product.
Example 6: in this embodiment, the MAX phase layered material with the A site being antimony and iron element is Ta 2 (Sb x Fe 1-x ) C powder material. The Ta 2 (Sb x Fe 1-x ) The preparation method of the powder C comprises the following steps:
(1) Weighing metal Ta powder with granularity of 500 meshes (purity of 99.99 wt.%) and FeSb with granularity of 300 meshes, wherein the molar ratio is 2:1:1 2 Powder (purity 99.99 wt.%) 300 meshAnd (3) grinding and mixing the materials to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1700 ℃, the heat preservation time is 120min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Crushing, grinding and sieving the reaction product to obtain a powder sample.
Example 7: in this embodiment, the MAX phase layered material with the A site being the antimony element is Nb 2 (Sb x Cu 1-x ) C powder material.
The Nb is 2 (Sb x Cu 1-x ) The preparation method of the powder C comprises the following steps:
(1) Weighing metal Nb powder (purity is 99.99 wt.%) with the granularity of 500 meshes and CuSb with 300 meshes, wherein the molar ratio is 2:1:1 2 Powder (purity 99.99 wt.%), 300 mesh graphite powder, and the above materials were ground and mixed to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1700 ℃, the heat preservation time is 120min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Crushing, grinding and sieving the reaction product to obtain a powder sample.
Example 8: in this embodiment, the MAX phase layered material with the A site being the antimony element is Ti 2 (Sb x Ni 1-x ) C powder material.
The Ti is 2 (Sb x Ni 1-x ) The preparation method of the powder C comprises the following steps:
(1) Weighing Ti with granularity of 500 meshes and molar ratio of 1:2:1:3:3 2 AlC powder, niCl 2 Powder (purity 99.99 wt.%), 300 mesh antimony powder (purity 99.99 wt.%), liCl (purity 99 wt.%), KCl (purity 99 wt.%) and the above materials were ground and mixed to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 400 ℃, the heat preservation time is 120min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, and after stirring and ultrasonic cleaning for 30 minutes, the remaining salt in the reaction product was washed away, followed by suction filtration. And (3) placing the reaction product obtained by suction filtration into a baking oven at 40 ℃, and taking out after 12 hours to obtain a powder product.
Example 9: in this embodiment, the MAX phase layered material with the A site being antimony element is Cr 2 (Sb x Co 1-x ) C powder material.
The Cr is 2 (Sb x Co 1-x ) The preparation method of the powder C comprises the following steps:
(1) Weighing Cr with granularity of 500 meshes and molar ratio of 1:3:1:10 2 AlC powder, coO powder (purity: 99.99 wt.%), 300 mesh antimony powder (purity: 99.99 wt.%), naI (purity: 99 wt.%) were ground and mixed to obtain a mixture. (2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 1000 ℃, the heat preservation time is 30min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, and after stirring and ultrasonic cleaning for 30 minutes, the remaining salt in the reaction product was washed away, followed by suction filtration. And (3) placing the reaction product obtained by suction filtration into a baking oven at 40 ℃, and taking out after 12 hours to obtain a powder product.
Example 10: in this embodiment, the MAX phase layered material with the A site being the antimony element is Ti 2 (Sb x Te 1-x ) C powder material.
The Ti is 2 (Sb x Te 1-x ) The preparation method of the powder C comprises the following steps:
(1) Weighing Ti with granularity of 500 meshes and molar ratio of 1:2.5:1:1:5 2 AlC powder and CdCl 2 Powder (purity 99.99 wt.%) 300 mesh antimony powder (purity99.99 wt.%), 300 mesh Te powder (purity 99.99 wt.%), naBr (purity 99 wt.%) and the above materials were ground and mixed to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 800 ℃, the heat preservation time is 50min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, and after stirring and ultrasonic cleaning for 30 minutes, the remaining salt in the reaction product was washed away, followed by suction filtration. And (3) placing the reaction product obtained by suction filtration into a baking oven at 40 ℃, and taking out after 12 hours to obtain a powder product.
Example 11: in this embodiment, the MAX phase layered material with the A site being the antimony element is V 2 SbC powder material.
The V is 2 The preparation method of SbC powder comprises the following steps:
(1) Weighing 500-mesh V with granularity of 1:3:1:6 by mol ratio 2 AlC powder, agCl powder (purity 99.99 wt.%), 300 mesh SnSb powder, naF (purity 99 wt.%) and grinding and mixing the above materials to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 800 ℃, the heat preservation time is 90min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, stirred and ultrasonically cleaned for 30 minutes, and then suction filtration was performed. And (3) treating the reaction product obtained by suction filtration with 2mol/L nitric acid solution, and washing out the residual metal simple substance in the reaction process. Finally, the reaction product after the treatment is filtered by suction and is cleaned by ethanol, and then is put into a baking oven at 40 ℃ and is taken out after 12 hours, thus obtaining the powder product.
Example 12: in this embodiment, the MAX phase layered material with the A site being the antimony element is Ti 3 (Sb x Sn 1-x )C 2 Powder material. The Ti is 3 (Sb x Sn 1-x )C 2 The preparation method of the powder comprises the following steps:
(1) Weighing 500-mesh Ti with granularity of 1:2:1:3 by mol ratio 3 AlC 2 Powder, coCl 2 Powder (purity 99.99 wt.%), 300 mesh SnSb powder, naCl (purity 99 wt.%) and the above materials were ground and mixed to obtain a mixture.
(2) The mixture was charged into an alumina crucible, and then placed into a high-temperature vacuum tube furnace for reaction. The reaction conditions are as follows: the reaction temperature is 800 ℃, the heat preservation time is 90min, and the inert atmosphere is protected. And after the sintering temperature is reduced to room temperature, taking out the reaction product in the alumina crucible.
(3) Washing the reaction product with deionized water and alcohol: the reaction product was placed in a beaker, deionized water was added, stirred and ultrasonically cleaned for 30 minutes, and then suction filtration was performed. And (3) treating the reaction product obtained by suction filtration with a 2mol/L hydrochloric acid solution, and washing out the residual metal simple substance in the reaction process. Finally, the reaction product after the treatment is filtered by suction and is cleaned by ethanol, and then is put into a baking oven at 40 ℃ and is taken out after 12 hours, thus obtaining the powder product.
The inventor also replaces the corresponding raw materials and process conditions in the previous examples 1-12 with other raw materials and process conditions described in the specification, and the results show that the MAX phase layered material containing the A-site antimony element can be obtained. Compared with the existing MAX phase material, the novel MAX phase material containing the A-site antimony element provided by the embodiment of the invention has a series of advantages of high strength, high heat conduction, high electric conduction, oxidation resistance, high temperature resistance, high damage tolerance, processability and the like, and the preparation process is simple and easy to operate, and has potential application prospects in the fields of superconducting, energy storage, catalysis, biology, microwave devices and the like.
While the invention has been described with reference to an illustrative embodiment, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (5)
1. A preparation method of a MAX phase layered material containing an antimony element at the A position is characterized by comprising the following steps: precursor MAX phase material, A and/or material containing A, metal fused salt and inorganic salt are mixed according to the proportion of 1: (1-3): (2-3): (3-10), and carrying out high-temperature reaction for 30-120 min at 400-1000 ℃ in an inert atmosphere, and then carrying out post-treatment to obtain the A-site MAX phase layered material containing antimony elements;
wherein the precursor MAX phase material is selected from Ti 3 AlC 2 、Ti 2 AlC、Ti 2 AlN、Ti 4 AlN 3 、V 2 AlC、Cr 2 AlC、Nb 2 AlC、Hf 2 AlN、Ta 4 AlC 3 、Ti 3 Any one or the combination of more than two AlCN; the A and/or A-containing material is selected from Sb, cdSb, ag 2 Sb、CoSb、Cu 2 Sb、FeSb、FeSb 2 Any one or a combination of two or more of NiSb, snSb, znSb;
the metal molten salt is selected from FeO and Fe 2 O 3 、CoO、NiO、CuO、ZnO、CdO、Ag 2 O、FeCl 2 、FeCl 3 、CoCl 2 、NiCl 2 、CuCl 2 、CuCl、ZnCl 2 、CdCl 2 、AgCl、FeBr 2 、FeBr 3 、CoBr 2 、NiBr 2 、CuBr 2 、CuBr、ZnBr 2 、CdBr 2 、AgBr、FeI 2 、CoI 2 、NiI 2 、CuI、ZnI 2 、CdI 2 、AgI、FeSO 4 、Fe 2 (SO 4 ) 3 、CoSO 4 、NiSO 4 、CuSO 4 、Cu 2 SO 4 、ZnSO 4 、CdSO 4 、Ag 2 SO 4 Either or both ofCombinations of the above;
the molecular formula of the MAX phase lamellar material is expressed as M n+1 AX n Wherein M is selected from any one or any combination of more than two of the elements in the front transition metal group, A is any combination of antimony or antimony-containing alloy, X is any one or any combination of two of the elements C, N, and n is 1,2, 3 or 4.
2. The method of manufacturing according to claim 1, characterized in that: and M comprises any one or any combination of more than two of Sc, ti, V, cr, mn, Y, zr, nb, mo, hf, ta, W.
3. The method of manufacturing according to claim 1, characterized in that: the inorganic salt is selected from any one or more than two of NaF, naK, liCl, naCl, KCl, naBr, KBr.
4. The method of manufacturing according to claim 1, characterized in that: x in the molecular formula of the MAX phase lamellar material is C x N y Wherein x+y=1 to 2.
5. The method of manufacturing according to claim 1, characterized in that: the MAX phase layered material containing antimony element at the A position has a hexagonal crystal system structure, and the space group is P6 3 /mmcThe unit cell is composed of M n+1 X n The substructure layer and the atomic layer containing antimony are alternately stacked.
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