Progress in Structural Tailoring and Properties of Ternary Layered Ceramics

doi:10.15541/jim20230123

Journal of Inorganic Materials ›› 2023, Vol. 38 ›› Issue (8): 845-884.DOI: 10.15541/jim20230123

Special Issue: 【材料计算】计算材料(202309)；【信息功能】Max层状材料、MXene及其他二维材料(202309)；【结构材料】核用陶瓷（202309）

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Progress in Structural Tailoring and Properties of Ternary Layered Ceramics

DING Haoming¹^,²^,³(), LI Mian¹^,³, LI Youbing¹^,³, CHEN Ke¹^,³, XIAO Yukun¹^,³, ZHOU Jie⁴, TAO Quanzheng⁴, Johanna Rosen⁴, YIN Hang⁵, BAI Yuelei⁵, ZHANG Bikun⁶, SUN Zhimei⁶, WANG Junjie⁷, ZHANG Yiming¹^,³, HUANG Zhenying⁸, ZHANG Peigen⁹, SUN Zhengming⁹, HAN Meikang¹⁰, ZHAO Shuang¹¹, WANG Chenxu¹¹, HUANG Qing¹^,³()

1. Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
2. University of Chinese Academy of Sciences, Beijing 101408, China
3. Qianwan Institute of CHiTECH, Ningbo 315336, China
4. Department of Physics, Chemistry and Biology (IFM), Linköping University, Linköping SE-58183, Sweden
5. National Key Laboratory of Science and Technology on Advanced Composites in Special Environments and Center for Composite Materials and Structures, Harbin Institute of Technology, Harbin 150001, China
6. School of Materials Science and Engineering, Beihang University, Beijing 100191, China
7. School of Materials Science and Engineering, Northwestern Polytechnic University, Xi’an 710072, China
8. School of Mechanical, Electronic and Control Engineering, Beijing Jiaotong University, Beijing 100044, China
9. School of Materials Science and Engineering, Southeast University, Nanjing 211189, China
10. Institute of Optoelectronics and Shanghai Frontiers Science Research Base of Intelligent Optoelectronics and Perception, Fudan University, Shanghai 200433, China
11. State Key Laboratory of Nuclear Physics and Technology, Peking University, Beijing 100871, China

Received:2023-03-09 Revised:2023-04-19 Published:2023-08-20 Online:2023-05-04
Contact: HUANG Qing, professor. E-mail: huangqing@nimte.ac.cn
About author:DING Haoming (1994-), male, PhD candidate. E-mail: dinghaoming@nimte.ac.cn
Supported by:
Key R&D Projects of Zhejiang Province(2022C01236);National Natural Science Foundation of China(12275009);National Natural Science Foundation of China(51972080);National Natural Science Foundation of China(52171033);National Natural Science Foundation of China(52272307);National Natural Science Foundation of China(21671195);National Natural Science Foundation of China(52172254);National Natural Science Foundation of China(U2004212);National Natural Science Foundation of China(52202325);Shanghai Pujiang Program(22PJ1400800);Leading Innovative and Entrepreneur Team Introduction Program of Zhejiang(2019R01003);Ten-Thousand Talents Plan of Zhejiang Province(2022R51007)

Abstract

Abstract:

MAX/MAB phases are a series of non-van der Waals ternary layered ceramic materials with a hexagonal structure, rich in elemental composition and crystal structure, and embody physical properties of both ceramics and metals. They exhibit great potential for applications in extreme environments such as high temperature, strong corrosion, and irradiation. In recent years, two-dimensional (2D) materials derived from the MAX/MAB phase (MXene and MBene) have attracted enormous interest in the fields of materials physics and materials chemistry and become a new 2D van der Waals material after graphene and transition metal dichalcogenides. Therefore, structural modulation of MAX/MAB phase materials is essential for understanding the intrinsic properties of this broad class of layered ceramics and for investigating the functional properties of their derived structures. In this paper, we summarize new developments in MAX/MAB phases in recent years in terms of structural modulation, theoretical calculation, and fundamental application research and provide an outlook on the key challenges and prospects for the future development of these layered materials.

Key words: MAX phase, MAB phase, MXene, structural modulation, theoretical calculation, review

CLC Number:

TB383

DING Haoming, LI Mian, LI Youbing, CHEN Ke, XIAO Yukun, ZHOU Jie, TAO Quanzheng, Johanna Rosen, YIN Hang, BAI Yuelei, ZHANG Bikun, SUN Zhimei, WANG Junjie, ZHANG Yiming, HUANG Zhenying, ZHANG Peigen, SUN Zhengming, HAN Meikang, ZHAO Shuang, WANG Chenxu, HUANG Qing. Progress in Structural Tailoring and Properties of Ternary Layered Ceramics[J]. Journal of Inorganic Materials, 2023, 38(8): 845-884.

Figures/Tables 28

Fig. 1 Non-exhaustive chronicle of ternary layered materials In 1960, Ti2SC was synthesized[40]; From 1960 to 1966, a large number of ternary layered carbides/nitrides (H-phases) with an M2AX formula (211 type) were synthesized[41-42]; From 1967 to 1968, Ti3SiC2 (312 type) and a set of 312 and 211 types H-phases were produced[41,43-44]; In 1969, a typical ternary layered boride Fe2AlB2 was synthesized[7]; In 1994, Ti3AlC2 was discovered[45]; In 1996, the high purity Ti3SiC2 was produced and exhibited excellent properties, thus triggering the research upsurge to these materials[46]; In 2000, Barsoum[1] renamed H-phases as Mn+1AXn phases, short for MAX phases; In 2011, the first MXene Ti3C2Tx was discovered[28]; In 2013, the discovery of magnetocaloric effect of Fe2AlB2 raised research upsurge on ternary layered borides[9]. Also, Lu2SnC was synthesized and found to be superconducting[47]; In 2014, an o-MAX (Cr2/3Ti1/3)3AlC2 was synthesized[48]; In 2015, ternary layered borides were named as MAB phases. In addition, the first Zr-based MAX phase was discovered[10,49]; In 2017, an i-MAX (Mo2/3Sc1/3)2AlC and two noble-metal MAX phases Ti3AuC2 and Ti3IrC2 were synthesized[22,50]; In 2019, a series of MAX phases containing Cu and Zn, and a hexagonal MAB phase Ti2InB2, as well as Nb2SBxC1-x (x=0-1) were synthesized[24⇓-26,51,52]; In 2020, two i-MAB phases (Mo2/3Sc1/3)2AlB2 and (Mo2/3Y1/3)2AlB2, as well as a variety of MAX phases containing Fe, Co, Ni, and Mn were synthesized[16,19]; In 2021, MAX phases having Se atoms at the A-site were produced[53]; In 2022, o-MAX phase Ti4MoSiB2, the first MBene, and Zr2Se(B1-xSex) were synthesized[20,54-55]; In 2023, a chemical scissor-mediated structural editing strategy was proposed, which extremely expands the diversity of MAX phases and MXene[56]

Fig. 2 Atomic and structural regulation of MAX phases (a) Schematic illustration of Ti3SiC2 film covered by Au film on the SiC substrate[22]; (b) STEM image of Ti3SiC2 and its corresponding atomic model[22]; (c) Schematic illustration of preparing novel MAX phases and MXene based on a Lewis-acidic-molten-salt route[24]; (d) STEM image of Ti3ZnC2 and its corresponding atomic model[24]; (e) STEM image of Ti3C2Cl2 and its corresponding atomic model[24]; (f) Schematic illustration of the conversion from non-van der Waals solids to 2D transition-metal chalcogenides[57]

Fig. 3 Different methods for the synthesis of MXene (a) Schematic illustration of preparing MXene using HF solution as etchant[28]; (b) SEM image of Ti3C2Tx prepared by HF solution, showing the typical accordion-like morpholorgy of MXene particle[28]; (c) STEM image of Ti3C2Cl2 prepared by Lewis-acidic-molten-salt route, and its corresponding atomic model[24]; (d) Schematic illustration of preparing Ti3C2Tx MXene via a reaction between Ti3SiC2 and CuCl2; (e) Redox potential/Gibbs free energy between Lewis acid cations and A-site atoms in molten salts[30]; (f) Schematic illustration of the electrochemistry etching strategy for the preparation of MXene in molten salt[72]

Fig. 4 Structural editing of MAX phases and MXene aided by chemical scissors (a) Schematic illustration of chemical intercalation strategy aided by chemical scissors[56]; (b) Periodic table showing elements involved in the formation of MAX phases and MXenes. Light blue: M elements; Brown: A elements; Black: X elements; Green: ligand (T) elements; Circled: elements studied in the present work[56]

Fig. 5 Crystal structure and physical properties of novel chalcogenide MAX phases (a-d) First synthesized Se-containing MAX phase, Zr2SeC[53]; (e, f) First synthesized Te-containing MAX phase, Hf2TeB[93]; (h-j) First synthesized MAX phase with chalcogen at X site, Zr2Se(B1-xSex) with x at 0 (h), 0.60 (i), and 0.97 (j), respectively[20]

Fig. 6 Preparation of single crystal MAX phases (a) Crystal structure of V4AlC3-x[106]; (b) SEM image of single MAX phase V4AlC3-x[106]; (c) Schematic of the experimental set-up used for high temperature solution growth[107]; (d) Photograph of part of the crucible cut after growth and dipping into dilute HCl, the Cr2AlC platelets are coalescing due to an unusually long growth time[107]

Fig. 7 Heat capacity and anisotropic thermal conductivity in Cr2AlC single crystals at high temperatures[110] (a) Atomic structure model of Cr2AlC; (b) Schematic of the in-plane resistivity measurements in Cr2AlC using a four-probe configuration with equidistant and parallel pads; (c) Temperature-dependence measurements of the in-plane resistivity for Cr2AlC single crystals (black line); (d) Predicted out-of-plane resistivity (orange line); (e) Heat capacity measurements of Cr2AlC single crystals measured experimentally (blue dots); (f) Measured in-plane (κ∥) and out-of-plane (κ⊥) thermal conductivities using various techniques

Fig. 8 i-MAX phases and its derived two-dimensional product of i-MXene[50] (a-c) i-MAX with in-plane chemical order, viewed from [100], [010] and [110] zone axes, respectively; (d) Schematic of the conversion from i-MAX to i-MXene; (e) Low-magnification STEM image of single flake of Mo1.33C i-MXene; (f) Higher magnification STEM image with the FFT result of Mo1.33C i-MXene; (g) Atomically resolved STEM image of Mo1.33C i-MXene; (h) Atomic structure model corresponding to (g)

Table 1 List of synthesized i-MAX phases

M′_4/3	M″_2/3	A	X	Ref.
Mo_4/3	Sc_2/3/Y_2/3	Al	C	[50,118]
W_4/3	Sc_2/3/Y_2/3	Al	C	[123]
Mn_4/3	Sc_2/3	Ga	C	[124]
Cr_4/3	Sc_2/3/Y_2/3/Zr_2/3	Al	C	[125-126]
Cr_4/3	Sc_2/3	Ga	C	[16,124]
V_4/3	Sc_2/3/Zr_2/3	Al	C	[118,127]
Mo_4/3	Sc_2/3/Y_2/3	Ga	C	[128]
Mo_4/3	Ce_2/3/Pr_2/3/Nd_2/3/Sm_2/3/Gd_2/3/Tb_2/3/Dy_2/3/Ho_2/3/Er_2/3/Tm_2/3/Lu_2/3	Al	C	[119]
Mo_4/3	Gd_2/3/Tb_2/3/Dy_2/3/Ho_2/3/Er_2/3/Tm_2/3/Yb_2/3/Lu_2/3	Ga	C	[120]
W_4/3	Gd_2/3/Tb_2/3/Dy_2/3/Ho_2/3/Er_2/3/Tm_2/3/Lu_2/3	Al	C	[121]
Cr_4/3	Gd_2/3/Tb_2/3/Dy_2/3/Ho_2/3/Er_2/3/Tm_2/3/Lu_2/3	Al	C	[122]

Fig. 9 MAB phases, i-MAB phases and o-MAB phases (a) SEM image of layered Ti2InB2; (b) STEM image of Ti2InB2 along the direction of [001] and corresponding FFT result in the inset image; (c) SEM image of 2D-TiB and its corresponding EDS semi-quantitative resultin inset table[52]; (d-f) STEM images of i-MAB phase (Mo2/3A1/3)2AlB2 and corresponding atomic model along the direction [0001], [$1\bar{1}00$] and [$11\bar{2}0$], respectively, and their corresponding FFT images[55]; (g-i) STEM images of o-MAB phase Ti4MoSiB2 and corresponding atomic model along the direction [100], [210] and [110], respectivly, and their corresponding FFT images[54]

Fig. 10 Two-dimensional products derived from MAB phases through chemical etching (a) Schematic of chemical etching i-MAB phase to prepare two-dimensional derivative[55]; (b) XRD patterns of prestine i-MAX (Mo2/3Y1/3)2AlB2, etched product Mo4/3B2-xTz, TBAOH intercalation product, and delamination film with SEM image (inset) showing the cross-sectional morphology of Mo4/3B2-xTz film [55]; (c) STEM image of monolayer Mo4/3B2-xTz and its FFT image (inset) [55]; (d) XRD patterns of o-MAX Ti4MoSiB2, product etched by ZnCl2 and two-dimensional TiOxCly after delamination and filtering with SEM image (inset) of cross-sectional morphology of a TiOxCly film[54]

Fig. 11 Experimentally measured unilateral notched beam fracture toughness as a function of the weakest to strongest chemical bond stiffness ratio kmin/kmax for some typical ternary layered compounds (MAX and MAB phases)[138]

Table 2 Stable MAB phases by theoretical prediction

MAB phase	M type	A type	Ref.	MAB phase	M type	A type	Ref.
Orthorhombic M₂A₂B₂	Ti	Al	[160-161]	Orthorhombic M₃AB₄	Sc	Al	[160-161]
	Hf				Ti
	V				Zr
	Nb				Hf
	Ta				V
	Tc				Nb
	Cr				Ta
	Mn				Mo
Orthorhombic M₂AB₂	Sc	Al	[160-161]		W
	Ti				Mn
	Zr				Fe
	Hf			Orthorhombic M₄AB₆	Sc	Al	[160-161]
	V				Ti
	Nb				Zr
	W				Hf
	Tc				V
	Rh				Nb
	Ni				Ta
	Co				Mo
Orthorhombic M₃A₂B₂	Sc	Al	[160-161]	Hexagonal M₂AB₂	Ti	Sn	[52]
	Ti				Hf	In	[162]
	Zr				Hf	Sn
	Hf				Zr	In
	Cr					Pb
	Mn					Tl
	Tc			Hexagonal M₃AB₄	Hf	In	[162]
	Fe					Sn
	Ni					P
					Zr	Cd
					Zr	Pb

Fig. 12 Theoretical calculation of MAB phases (a) Structures of orthorhombic and hexagonal MAB phases[163]; (b) Bonding energy of M2AlB2-type orthorhombic MAB and M2AlC-type MAX phases; (c) Simulated exfoliation process of orthorhombic M2AlB2 using HF, where the red, green, black, cyan, and pink balls represent Mo, B, Al, F, and H atoms, respectively[146]

Table 3 Theoretical mechanical properties of several MAB-phases, including bulk modulus (B), shear modulus (G), Young’s modulus (E), and Poisson ratio (ν)

MAB phase	B/GPa	G/GPa	E/GPa	¯ν/GPa	Ref.
Mn₂AlB₂	239	169	411	0.21	[160]
Fe₂AlB₂	209	133	329	0.24
Co₂AlB₂	216	92	242	0.31
TiAlB	145	116	274	0.18
VAlB	173	133	317	0.19
NbAlB	180	130	315	0.21
TaAlB	192	138	333	0.21
CrAlB	189	140	338	0.20
MnAlB	167	101	252	0.25
TcAlB	220	114	292	0.28
Sc₂AlB₂	238	142	356	0.25
Ti₂AlB₂	170	150	347	0.16
Zr₂AlB₂	152	112	270	0.20
Hf₂AlB₂	168	132	314	0.19
V₂AlB₂	195	129	317	0.23
Nb₂AlB₂	199	110	279	0.27
Cr₂AlB₂	229	177	422	0.19
Mo₂AlB₂	238	142	356	0.25
W₂AlB₂	262	139	354	0.28
Tc₂AlB₂	260	132	339	0.28
Ni₂AlB₂	200	91	237	0.30
MoAlB	213	146	357	0.22	[164]
WAlB	232	146	362	0.24	[164]
Mn₂AlB₂	222	161	388	0.21	[165]
Fe₂AlB₂	210	132	329	0.24	[165]
Co₂AlB₂	241	101	266	0.31	[166]
Zr₃CdB₄	—	82	202	0.37	[167]
Hf₃PB₄	—	180	407	0.19	[168]

Fig. 13 Members and atomic structures of all reported orth- and hex-MBenes[163]

Fig. 14 Discovery of ternary MAX phases (a) Calculation-based approach to discovery of novel ternary phases Ti2InB2[52]; (b) High-throughput prediction of MAB phases[162]; (c) Crystal structures for the stable Nb2AB2 and Nb2AB (A: P or S)[183]

Fig. 15 Theoretical study of quaternary MAB phases (a) Crystal structure of Cr3AlB4, ordered M2M'AlB4, and disordered M2M'AlB4[186]; (b) Prediction and synthesis of i-MAB phases Mo4/3Sc2/3AlB2 and Mo4/3Y2/3AlB2[16]; (c) Elemental mapping involved in this computational work; (d) Schematic illustration of the evolution of structure and electronic structure of h-MAB during the introduction of the fourth element M″[187]

Fig. 16 Structure mapping based on the selected characteristic quantities of electron concentration and atomic sizes[36]

Fig. 17 MAX-reinforced metal matrix composites (a-b) Fracture morphology of MAX in Mg matrix composites undergoing microplastic deformation[213]; (c) MAX/Cu matrix composite MCC pantograph slide plate[215]; (d, e) Transformation of MAX to TiCx and Cr3C2 in Ni matrix composites and morphology of in situ authentic γ'[224]; (f) Morphology of the MAX transformation to TiCx and Ti5Si3 in Ti matrix composites[225]

Fig. 18 SEM images of a Sn whisker alternately cultivated in air and vacuum[259] (a-e) For once, twice, 3 times, 4 times, and 5 times, respectively with faceted segments formed in vacuum being pointed by white arrows; (f-h) High magnification SEM images of the faceted segments indicated by arrow A in (b), arrow C in (c), and arrow C in (d), respectively

Fig. 19 SEM images of fractured Zr2InC surface and an In whisker[243] (a) Fractured Zr2InC surface showing In at grain boundaries (this surface being covered with thin In film); (b) An In whisker whose cross-sectional shape is determined by grain boundary geometry at the In/Zr2InC interface

Fig. 20 Microstructure of Sn whiskers/Ti2SnC interface[266] (a) TEM image of the interface; (b) Magnified view of the white rectangle area in (a); (c, d) HRTEM images of the interface

Fig. 21 (a) Electrical conductivity of different MXene films and (b) conductivity-dependent electromagnetic interference shielding effectiveness of different MXenes[282]

Fig. 22 Defect generation and microstructural transformation in MAX phase materials under irradiation (a) STEM HAADF (high-angle annular dark-field) image along [11¯20] of Ti3AlC2 irradiated with 1 MeV Au ions, showing direct evidence of cation antisite defects. The white arrows indicate the initial Al layers, whose image contrast is altered when compared with the initial hexagonal structure[295]; (b, c) Contrast profiles along line 1 and line 2 in (a), respectively, which directly show the variation of contrast arising from the formation of TiAl-AlTi antisite defects produced by ion irradiation[295]; (d) TEM image of Ti3(Si,Al)C2 being irradiated at 0.2 dpa indicating a cluster of point defects (black dots)[296]; (e-g) Phase transformation (hcp to γ to fcc solid solution) processes with chemical disorder induced by ion irradiation in a typical MAX phase, Ti3AlC2 (hcp: hexagonal close packing; fcc: face-centered cubic)[295]

Fig. 23 MAX phase irradiation temperature effect (a) Ti3AlC2 is completely recovered to initial phase (a dose of 2×1016 cm-2) or partially recovered to initial phase and γ-Ti3AlC2 phase (a dose of 4×1016 cm-2) after irradiation with 1 MeV Au ions and then annealed at 800 ℃ for 1 h[303]; (b) Cr2AlC films showing completely amorphous after irradiation with 320 keV Xe ions up to 3.3 dpa at 300 K, but not completely amorphized after irradiation up to 90 dpa at 623 K[306]

Fig. 24 Phase transformation and amorphization caused by irradiation of MAX phases[302] (a) Schematic of atomic structure models of Ti2SnC and (TiVNbZrHf)2SnC; (b) In-situ selective area electron diffraction (SAED) micrographs of Ti2SnC and five-component (TiVNbZrHf)2SnC recorded during 800 keV Kr2+ irradiation, showing different phase transformation process and amorphization resistance; (c) M-Sn antisite defect formation energies calculated via DFT in the corresponding single-component M2SnC and the five-component (TiVNbZrHf)2SnC supercell

Fig. 25 STEM micrographs of (Mo2/3RE1/3)2GaC i-MAX phase along (a) [100] and (b) [010] zone axis[120]

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Progress in Structural Tailoring and Properties of Ternary Layered Ceramics

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