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Sulfur-series medium-high entropy MAX phase solid solution material as well as preparation method and application of same

A technology of solid solution and powder materials, applied in the field of sulfur-based high-entropy MAX phase solid solution materials and their preparation, and MAX phase solid solution materials, can solve the problems of simple sulfur being volatile and unstable, difficult to synthesize, etc., and achieve good application prospects. The method is simple and easy, and the effect of reducing pollution

Inactive Publication Date: 2020-12-18
宁波材料所杭州湾研究院 +1
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  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide a kind of medium high entropy MAX phase solid solution material of sulfur system and its preparation method, thereby overcome the deficiencies in the prior art, solve the high temperature required for the synthesis of high entropy MAX phase in sulfur system, and the volatile elemental sulfur source Unstable, it is difficult to synthesize a higher purity target phase

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  • Sulfur-series medium-high entropy MAX phase solid solution material as well as preparation method and application of same
  • Sulfur-series medium-high entropy MAX phase solid solution material as well as preparation method and application of same
  • Sulfur-series medium-high entropy MAX phase solid solution material as well as preparation method and application of same

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preparation example Construction

[0035] Another aspect of the embodiments of the present invention provides a method for preparing a sulfur-based medium-high entropy MAX phase solid solution material, comprising: providing ferrous sulfide as a high-temperature solid sulfur source;

[0036] React the mixture containing the ferrous sulfide, transition metal elemental substance and / or transition metal hydride and transition metal carbide at 1400-1800°C for 10-30 minutes to obtain the sulfur-based medium-high entropy MAX phase solid solution material, whose chemical formula is m 2 SC, where M includes any combination of three or more of Ti, Zr, Hf, V, Nb, and Ta.

[0037] In some embodiments, the preparation method specifically includes:

[0038] Mixing ferrous sulfide, transition metal elemental substance and / or transition metal hydride and transition metal carbide according to the molar ratio of (1.0~1.2):(1.9~2.1):(0.8~1) to obtain a mixture;

[0039] Using a spark plasma sintering system, raise the temperat...

Embodiment 1

[0055] In this embodiment, the entropy MAX phase solid solution material in the sulfur series is (Ti, Zr, Hf) 2 SC. The preparation steps of the solid solution material are as follows:

[0056] (1) Choose titanium carbide, zirconium, zirconium carbide, hafnium hydride and ferrous sulfide as raw materials, according to TiC: Zr: ZrC: HfH 2 : The molar ratio of FeS is 2:1:1:2:3.2, mixed with alcohol as the medium for 30min during grinding, and dried in a vacuum oven. In this embodiment, if hafnium is easily oxidized, the use of hafnium hydride is beneficial to improve the purity of the target phase.

[0057] (2) Using a spark plasma sintering system, heat preservation at 1600°C for 20min at a heating rate of 50°C / min.

[0058] (3) The powder obtained in step (2) is crushed and ground to 300 mesh to obtain a precursor powder with uniform particle size distribution.

[0059] (4) Select dilute hydrochloric acid aqueous solution with a concentration of 3 mol / L as the etchant, etc...

Embodiment 2

[0065] In this embodiment, the sulfur-based high-entropy MAX phase solid solution material is (Ti, Zr, Hf, V) 2 SC. The preparation steps of the solid solution material are as follows:

[0066] (1) Choose titanium carbide, zirconium, hafnium hydride, vanadium carbide and ferrous sulfide as raw materials, according to TiC: Zr: HfH 2: The molar ratio of VC: FeS is 2:2:2:2:4.2, mixed with alcohol for 30min in the grinding process, and dried in a vacuum oven.

[0067] (2) Using a spark plasma sintering system, heat preservation at 1600°C for 20min at a heating rate of 50°C / min.

[0068] (3) The powder obtained in step (2) is crushed and ground to 300 mesh to obtain a precursor powder with uniform particle size distribution.

[0069] (4) Select dilute hydrochloric acid aqueous solution with a concentration of 3 mol / L as the etchant, etch at 50° C. for 2 days, and fully magnetically stir.

[0070] (5) Use polyvinylidene fluoride microporous filter membrane (PVDF, 0.45 μ m in por...

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Abstract

The invention discloses a sulfur-series medium-high entropy MAX phase solid solution material as well as a preparation method and application of the same, wherein the M position of the sulfur-series medium-high entropy MAX phase solid solution material comprises any three or a combination of more than four of transition metal elements Ti, Zr, Hf, V, Nb and Ta, the A position is a sulfur element, and the X position is a carbon element. The preparation method comprises the steps that ferrous sulfide serves as a high-temperature solid sulfur source, transition metal sulfide is obtained through areplacement reaction between transition metal simple substances and the ferrous sulfide, then the transition metal sulfide reacts with metal carbide, and the sulfur-series medium-high entropy MAX phase solid solution material is obtained. The ferrous sulfide sulfur source and the sulfur-containing intermediate product adopted by the invention are both stable metal sulfides, so that volatilizationof elemental sulfur in the high-temperature preparation process is avoided, and the synthesis path of a target phase is favorably controlled. The sulfur-series medium-high entropy MAX phase solid solution material is expected to have a good application prospect in the field of extreme environment structural materials such as nuclear power and high-speed rails.

Description

technical field [0001] The invention relates to a MAX phase solid solution material, in particular to a sulfur-based medium and high-entropy MAX phase solid solution material and its preparation method and application, belonging to the technical field of ternary layered compound MAX phase materials. Background technique [0002] The MAX phase is a nanolayered ternary compound with structural and performance diversity, exhibiting a hexagonal symmetric structure (P6 3 / mmc), with M n+1 AX n molecular formula. Wherein, M is a former transition group metal, A is usually IIIA and IVA group elements, X is carbon or nitrogen, and n is mostly 1-3 (M.W.Barsoum et al., Prog.Solid State Chem., 2000, 28, 201 -281). It is generally believed that the crystal structure of the MAX phase is determined by the M n+1 x n Nanostructured sublayers and A-site monoatomic layers are stacked alternately. Among them, M n+1 x n covalently bonded edge-shared M 6 The X octahedral layer is compo...

Claims

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Application Information

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IPC IPC(8): C04B35/547C04B35/626
CPCC04B35/547C04B35/626C04B2235/3843C04B2235/404C04B2235/3839C04B2235/44
Inventor 黄庆陈科周小兵宋育杰周洁
Owner 宁波材料所杭州湾研究院
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