CN108910884A - A kind of novel MAX phase material, preparation method and application - Google Patents
A kind of novel MAX phase material, preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of novel MAX phase materials and preparation method thereof.The molecular formula of the novel MAX phase material is expressed as Mn+ 1AhXn, M is selected from III B, any one in IV B, V B, VI B race element or two or more combinations, A are Zn element, and X is C element and/or N element, and n 1,2,3 or 4, h is positioned at Mn+1XnThe number of plies of A layer atom between elementary layer, and h is 1,2 or 3.The MAX phase material has hexagonal system structure, and space group P63/mmc, structure cell is by Mn+1XnUnit and AhLayer atom alternating stacking forms.Novel MAX phase material of the invention has application prospect in fields such as aerospace thermal structure material, nuclear energy structural material, high temperature electrode, fretting wear, energy storage.
Description
Technical field
The present invention relates to a kind of composite inorganic materials, and in particular to a kind of novel MAX phase material belongs to material technology neck
Domain.
Background technique
MAX phase is a kind of ternary compound with microcosmic layer structure, molecular formula Mn+1AXn, wherein M be III B,
IV B, V B, VI B race early transition metal element, A is mainly III A, IV A race element, and X is carbon or nitrogen, n=1~3.MAX phase
Material has hexagonal crystal system, and space group P63/mmc, structure cell is by Mn+1XnUnit replaces stacking with A atomic plane and forms, n=1,
2 or 3, often referred to simply as 211,312 and 413 phases.MAX phase has high intensity, high tenacity, high heat conductance, low irradiation active, excellent
Damage tolerance and thermal shock resistance, and characteristics such as high temperature resistant, anti-oxidant, easy processing, in aerospace thermal structure material, height
There is potential application in the fields such as warm electrode, fretting wear, nuclear energy structural material, energy storage.
Being studied the MAX phase material that is synthesized at present, there are about more than 70.But the A bit element one of existing MAX phase material
It directly is confined to the element that main group III A and IV A are covered, in particular, the position the A atom of actually major part MAX phase material is Al member
Element.And the change of A bit element, MAX can be caused to coordinate the change of bond strength, electronic structure, thus further to its physical chemistry
Performance causes deep effect.Therefore the existence range for extending MAX phase material A bit element, explores novel MAX phase material, has
Important theoretical and practical significance.
Existing MAX phase material preparation process is solid sintering technology, i.e., will several element powders such as M, A, X mix after heat into
Row pyroreaction, but the MAX phase material type that this method can be prepared is limited, and A therein is only limited to Al, Si above-mentioned etc. III
A, IV A race element.Although there is researcher to attempt A bit element replacing with the other elements such as Zn, and using solid sintering technology into
The preparation of the corresponding MAX phase material of row, however in solid-phase sintering process, the A bit such as Zn element are easily anti-with the M bit element such as Ti, V, Cr
Alloy phase should be generated, and the thermodynamic stability of the alloy phase is much higher than target MAX phase, i.e., alloy, which is met, is preferentially produced, so that A
Bit element is that the MAX phase material of Zn can not be formed.So far, it there is no the report in relation to the MAX phase material that A bit element is Zn.
Summary of the invention
The main purpose of the present invention is to provide a kind of novel MAX phase material, preparation method and applications, to overcome existing
There is the deficiency in technology.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes：
The embodiment of the invention provides a kind of novel MAX phase material, molecular formula is expressed as Mn+1AhXn, wherein M is selected from III
Any one in B, IV B, V B, VI B race element or two or more combinations, A is Zn element, in X C, N element
The combination of any one or two kinds, n 1,2,3 or 4, h 1,2 or 3.
Further, the M preferably includes any one in Sc, Ti, V, Cr, Zr, Nb, Mo, Hf, Ta or two
Kind or more combination.
Further, the X can be preferably CxNy, wherein x+y=1.
Further, the MAX phase material has hexagonal system structure, and space group P63/mmc, structure cell is by Mn+1XnIt is single
Member and AhLayer atom alternating stacking forms.
Further, the form of the MAX phase material include powder, block, in film any one or it is two or more
Combination, and it is without being limited thereto.
The embodiment of the invention also provides a kind of preparation methods of novel MAX phase material, it is characterised in that including：
Presoma MAX phase material, Zn and/or material containing Zn, inorganic salts are pressed 1：1.5~3：3~6 molar ratio mixing,
And by obtained mixture in inert atmosphere in 400 DEG C~1000 DEG C progress pyroreactions, post-processed later, obtain it is novel
MAX phase material；
The molecular formula of the presoma MAX phase material is expressed as Mm+1A’Xm, wherein M is selected from III B, IVB, V B or VI B
The early transition metal element of race, A ' are selected from III A or IV A race element, and X includes C and/or N, m=1,2 or 3.
Further, the presoma MAX phase material includes Ti3AlC2、Ti3SiC2、Ti2AlC、Ti2AlN、Ti4AlN3、
Ti2GaC、V2AlC、V2GaC、Cr2GaN、Cr2AlC、Sc2AlC、Zr2AlC、Zr2SnC、Nb2AlC、Nb4AlC3、Mo2AlC、
Mo2GaN、Hf2AlC、Hf2AlN、Ta3AlC2、Ta4AlC3In any one or two or more combinations, but not limited to this.Into
One step, the material containing Zn includes ZnO, ZnCl2、ZnBr2、ZnSO4In any one or two or more combinations, but not
It is limited to this.
Further, the inorganic salts include any one or two kinds in NaF, NaK, NaCl, KCl, NaBr, KBr with
On combination, but not limited to this.
Further, the presoma MAX phase material be powder, block, in film any one or it is two or more
Combination, but not limited to this.
Further, the Zn and/or material containing Zn are powder, and granularity is 500nm-50 μm.
Further, the inorganic salts are powder, and partial size is 500nm-1mm.
In some embodiments, the post-processing includes：After the pyroreaction, with deionized water pair
The reaction product obtained is cleaned, and later in 60-100 DEG C of drying, obtains the novel MAX phase material.
The embodiment of the invention also provides the novel MAX phase materials in preparation aerospace thermal structure material, nuclear energy knot
Purposes among structure material, high-temperature electrode material, fretting wear material or energy storage material etc..
Compared with the prior art, advantages of the present invention at least that：
(1) it is Zn element that the preparation method of novel MAX phase material provided in an embodiment of the present invention realizes A bit element for the first time
MAX phase material preparation, and it is simple to operation, there is universality；
(2) novel MAX phase material A bit element provided in an embodiment of the present invention is Zn element, and electronic structure is compared to existing
There is MAX phase material that biggish variation has occurred, the physicochemical properties which will lead to MAX phase material change, to it
Application in fields such as aerospace thermal structure material, nuclear energy structural material, energy storage generates deep effect.
Detailed description of the invention
Fig. 1 is MAX phase material Ti in the embodiment of the present invention 13ZnC2And tradition MAX phase material Ti3AlC2XRD spectra.
Fig. 2 is MAX phase material Ti in the embodiment of the present invention 13ZnC2Along the high-resolution-ration transmission electric-lens figure of different crystal zone axis.
Fig. 3 a is MAX phase material Ti in the embodiment of the present invention 13ZnC2Energy spectrum analysis figure under high-resolution-ration transmission electric-lens.
MAX phase material Ti in Fig. 3 b embodiment of the present invention 13ZnC2Cell configuration schematic diagram.
Fig. 4 is MAX phase material Ti in the embodiment of the present invention 13ZnC2Scanning electron microscope (SEM) photograph.
Fig. 5 is MAX phase material Ti in the embodiment of the present invention 22The XRD spectra of ZnC.
Fig. 6 is MAX phase material Ti in the embodiment of the present invention 22High-resolution-ration transmission electric-lens figure of the ZnC along different crystal zone axis.
Fig. 7 is MAX phase material Ti in the embodiment of the present invention 22Energy spectrum analysis figure of the ZnC under high-resolution-ration transmission electric-lens.
Fig. 8 is MAX phase material Ti in the embodiment of the present invention 32The XRD spectra of ZnN.
Fig. 9 is MAX phase material Ti in the embodiment of the present invention 32High-resolution-ration transmission electric-lens figure of the ZnN along different crystal zone axis.
Figure 10 is MAX phase material Ti in the embodiment of the present invention 32Energy spectrum analysis figure of the ZnN under high-resolution-ration transmission electric-lens.
Figure 11 is MAX phase material V in the embodiment of the present invention 42The XRD spectra of ZnC.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail, it should be pointed out that embodiment described below purport
It is being convenient for the understanding of the present invention, and is not playing any restriction effect to it.
Embodiment 1：In the present embodiment, novel MAX phase material is Ti3ZnC2, presoma MAX phase is Ti3AlC2, material containing Zn
Expect to be Zn powder, inorganic salts NaCl, these raw materials can be obtained by the approach such as commercially available.The Ti3ZnC2Preparation method such as
Under：
(1) NaCl 5.84g, the Ti that 10 μm of granularity are weighed3AlC2Powder 6g, 300 mesh Zn powder 3g grind above-mentioned material mixed
It closes, obtains mix products.
(2) mixture is placed in corundum crucible, is put into high temperature process furnances and is reacted.Reaction condition is：800 DEG C,
30 minutes, argon gas protection.After tubular type furnace temperature drops to room temperature, crucible reaction product is taken out.
(3) reaction product is washed with deionized：Reaction product is put into beaker, deionized water is added, stirs and surpasses
Sound stands 1 hour after cleaning 30 minutes, outwells supernatant.Washing reaction product three times after, put it into 80 DEG C of baking oven, 24
It is taken out after hour, obtains solid product.
Fig. 1 is solid product Ti obtained above3ZnC2XRD spectrum and tradition MAX phase material Ti3AlC2Comparison.It is logical
Comparison is crossed as can be seen that the XRD spectrum peak type of the two is integrally similar, has apparent (002), (004), (006) etc. along (00l)
The diffraction maximum of planar orientation both shows in crystal growing process preferential all to look unfamiliar length, and then the table on microscopic appearance along (00l)
Reveal layer structure.Ti can be determined by the position of (002) face diffraction maximum3ZnC2The c value of lattice constant is 1.87nm, the value
With Ti3ZnC2The c value 1.857nm of lattice constant is close.The difference of the two XRD spectrum is：1),(002),(004),(006),
(101), the intensity of the diffraction maximums such as (103) is different, which is because of Ti3ZnC2And Ti3AlC2The position A atom it is different, the two is brilliant
Lattice are different to the scattering power of X-ray；2), the diffraction maximums position such as (104), (105), (110) is different, the phenomenon be because
Ti3ZnC2And Ti3AlC2The position A atom it is different, the lattice parameter of the two is different.XRD data have absolutely proved the present embodiment preparation
Obtained Ti3ZnC2Material crystal structure and Ti3AlC2It is similar, it is the ternary layered MAX phase with the space P63/mmc group structure
Material.
Fig. 2 is the Ti observed along different crystal zone axis3ZnC2High-resolution-ration transmission electric-lens pattern, can be bright by the figure
Aobvious finds out Ti3ZnC2Layered crystal structure, the higher layer of brightness is the higher Zn atomic layer of atomic number in figure, brightness compared with
Low layer is Ti3C2Layer.
Fig. 3 a is under high-resolution-ration transmission electric-lens to Ti3ZnC2The Morphology analysis of progress, can be more clear by the figure
Clear finds out Ti3ZnC2Lattice by Zn atomic layer and Ti3C2Alternately stacking forms layer.Fig. 3 b is Ti3ZnC2Cell configuration show
It is intended to.
Embodiment 2：In the present embodiment, novel MAX phase material is Ti2ZnC, presoma MAX phase is Ti2GaC, material containing Zn
For ZnSO4, inorganic salts KCl, these raw materials can obtain by the approach such as commercially available.The Ti2The preparation method of ZnC is as follows：
(1) KCl 7.45g, the Ti that 10 μm of granularity are weighed2GaC powder 4g, ZnSO4Powder 5.4g, by above-mentioned material ground and mixed,
Obtain mix products.
(2) mixture is placed in corundum crucible, is put into high temperature process furnances and is reacted.Reaction condition is：700 DEG C,
30 minutes, argon gas protection.After tubular type furnace temperature drops to room temperature, crucible reaction product is taken out.
(3) reaction product is washed with deionized：Reaction product is put into beaker, deionized water is added, stirs and surpasses
Sound stands 1 hour after cleaning 30 minutes, outwells supernatant.Washing reaction product three times after, put it into 80 DEG C of baking oven, 24
It is taken out after hour, obtains solid product.
Fig. 5 is solid product Ti obtained above2The XRD spectrum of ZnC.Ti2The XRD spectrum of ZnC have apparent (002),
(004), (006) diffraction maximum, shows Ti2ZnC has preferable degree of orientation along the face (00l).Wherein (002) diffraction peak in
Near 13 °, corresponding lattice constant c value is about 1.362nm, with Ti2The 211 type MAX such as AlC is close.
Fig. 6 is the Ti observed along different crystal zone axis2The high-resolution-ration transmission electric-lens pattern of ZnC, can be bright by the figure
Aobvious finds out Ti2The layered crystal structure of ZnC, the higher layer of brightness is the higher Zn atomic layer of atomic number in figure, brightness compared with
Low layer is Ti2C layers.
Fig. 7 is under high-resolution-ration transmission electric-lens to Ti2The Morphology analysis that ZnC is carried out, can be more clear by the figure
Clear finds out Ti2The lattice of ZnC is by Zn atomic layer and Ti2C layers of alternating stacking form.
Embodiment 3：In the present embodiment, novel MAX phase material is Ti2ZnN, presoma MAX phase is Ti2AlN, material containing Zn
For Zn powder, inorganic salts NaBr, these raw materials can be obtained by the approach such as commercially available.The Ti2The preparation method of ZnN is as follows：
(1) NaBr 10.3g, the Ti that 20 μm of granularity are weighed2AlN powder 4.2g, 300 mesh Zn powder 3g grind above-mentioned material mixed
It closes, obtains mix products.
(2) mixture is placed in corundum crucible, is put into high temperature process furnances and is reacted.Reaction condition is：1100 DEG C,
30 minutes, argon gas protection.After tubular type furnace temperature drops to room temperature, crucible reaction product is taken out.
(3) reaction product is washed with deionized：Reaction product is put into beaker, deionized water is added, stirs and surpasses
Sound stands 1 hour after cleaning 30 minutes, outwells supernatant.Washing reaction product three times after, put it into 80 DEG C of baking oven, 24
It is taken out after hour, obtains solid product.
Fig. 8 is solid product Ti obtained above2The XRD spectrum of ZnN.Ti2The XRD spectrum of ZnN have apparent (002),
(004), (006) diffraction maximum, shows Ti2ZnC has preferable degree of orientation along the face (00l).Wherein (002) diffraction peak in
Near 13 °, corresponding lattice constant c value is about 1.354nm, with Ti2The 211 type MAX such as AlN is close.
Fig. 9 is the Ti observed along different crystal zone axis2The high-resolution-ration transmission electric-lens pattern of ZnN, can be bright by the figure
Aobvious finds out Ti2The layered crystal structure of ZnN, the higher layer of brightness is the higher Zn atomic layer of atomic number in figure, brightness compared with
Low layer is Ti2N layers.
Figure 10 is under high-resolution-ration transmission electric-lens to Ti2The Morphology analysis that ZnN is carried out, can be more clear by the figure
Clear finds out Ti2The lattice of ZnN is by Zn atomic layer and Ti2N layers of alternating stacking form.
Embodiment 4：In the present embodiment, novel MAX phase material is V2ZnN, presoma MAX phase is V2AlC, material containing Zn are
Zn powder, inorganic salts NaCl, these raw materials can be obtained by the approach such as commercially available.The V2The preparation method of ZnN is as follows：
(1) NaC 5.84g, the V that 10 μm of granularity are weighed2AlC powder 4.34g, 300 mesh Zn powder 3g grind above-mentioned material mixed
It closes, obtains mix products.
(2) mixture is placed in corundum crucible, is put into high temperature process furnances and is reacted.Reaction condition is：800 DEG C,
30 minutes, argon gas protection.After tubular type furnace temperature drops to room temperature, crucible reaction product is taken out.
(3) reaction product is washed with deionized：Reaction product is put into beaker, deionized water is added, stirs and surpasses
Sound stands 1 hour after cleaning 30 minutes, outwells supernatant.Washing reaction product three times after, put it into 80 DEG C of baking oven, 24
It is taken out after hour, obtains solid product.
Figure 11 is solid product V obtained above2The XRD spectrum of ZnC.V2The XRD spectrum of ZnC have apparent (004),
(006) diffraction maximum shows V2ZnC has preferable degree of orientation along the face (00l).Wherein (004) diffraction peak is near 26 °,
Corresponding lattice constant c value is about 1.323nm, with V2The 211 type MAX such as AlC is close.
In addition, other raw materials and process conditions substitution previous embodiment 1-4 that inventor is also addressed with this specification
In corresponding raw material and process conditions carried out related experiment, as a result show, the novel MAX phase based on Zn element can be obtained
Material.It is summarized, compared with existing MAX phase material, the novel MAX phase material that present invention provides has high-strength out
Degree, high thermal conductivity, high damage tolerance and the series of advantages such as processable, and preparation process is simple to operation, in aerospace heat knot
The fields such as structure material, nuclear energy structural material, energy storage have application prospect.
It should be appreciated that the above description is only an embodiment of the present invention, it is not intended to limit the scope of the invention, it is all
Using equivalent structure or equivalent flow shift made by description of the invention and accompanying drawing content, it is applied directly or indirectly in other
Relevant technical field, is included within the scope of the present invention.
Claims (10)
1. a kind of novel MAX phase material, it is characterised in that：The molecular formula of the MAX phase material is expressed as Mn+1AhXn, wherein M is selected
From any one or the two or more combinations in III B, IV B, V B, VI B race element, A is Zn element, and X C, N are first
The combination of any one or two kinds in element, n 1,2,3 or 4, h are positioned at Mn+1XnThe number of plies of A layer atom between elementary layer,
And h is 1,2 or 3.
2. novel MAX phase material according to claim 1, it is characterised in that：The M include Sc, Ti, V, Cr, Zr,
Any one in Nb, Mo, Hf, Ta or two or more combinations.
3. novel MAX phase material according to claim 1, it is characterised in that：The X is CxNy, wherein x+y=1.
4. novel MAX phase material according to claim 1, it is characterised in that：The MAX phase material has hexagonal crystal tying
Structure, space group P63/mmc, structure cell is by Mn+1XnUnit and AhLayer atom alternating stacking forms.
5. novel MAX phase material according to claim 1, it is characterised in that：The form of the MAX phase material includes powder
Body, block, any one or two or more combinations in film.
6. the preparation method of novel MAX phase material described in any one of claim 1-5, it is characterised in that including：
Presoma MAX phase material, Zn and/or material containing Zn, inorganic salts are pressed 1：1.5~3：3~6 molar ratio mixing, and will
Obtained mixture, in 400 DEG C~1000 DEG C progress pyroreactions, is post-processed later in inert atmosphere, obtains novel MAX
Phase material；
The molecular formula of the presoma MAX phase material is expressed as Mm+1A’Xm, wherein M is selected from III B, IVB, V B or VI B race
Early transition metal element, A ' are selected from III A or IV A race element, and X includes C and/or N, m=1,2 or 3.
7. preparation method according to claim 6, it is characterised in that：The presoma MAX phase material includes Ti3AlC2、
Ti3SiC2、Ti2AlC、Ti2AlN、Ti4AlN3、Ti2GaC、V2AlC、V2GaC、Cr2GaN、Cr2AlC、Sc2AlC、Zr2AlC、
Zr2SnC、Nb2AlC、Nb4AlC3、Mo2AlC、Mo2GaN、Hf2AlC、Hf2AlN、Ta3AlC2、Ta4AlC3In any one or two
Kind or more combination；And/or the material containing Zn includes ZnO, ZnCl2、ZnBr2、ZnSO4In any one or it is two or more
Combination；And/or the inorganic salts include in NaF, NaK, NaCl, KCl, NaBr, KBr any one or it is two or more
Combination.
8. preparation method according to claim 6 or 7, it is characterised in that：The presoma MAX phase material is powder, block
Any one in body, film or two or more combinations；And/or the Zn and/or material containing Zn are powder, and granularity is
500nm-50μm；And/or the inorganic salts are powder, and partial size is 500nm-1mm.
9. preparation method as claimed in claim 7, which is characterized in that the post-processing includes：In the pyroreaction
After, the reaction product obtained is cleaned with deionized water, later in 60-100 DEG C of drying, obtains the novel MAX
Phase material.
10. novel MAX phase material described in any one of claim 1-5 is in preparation aerospace thermal structure material, nuclear energy structure
Purposes in material, high-temperature electrode material, fretting wear material or energy storage material.
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| CN201810751303.5A CN108910884B (en) | 2018-07-10 | 2018-07-10 | MAX phase material, preparation method and application thereof |
| US16/977,097 US20200407281A1 (en) | 2018-07-10 | 2018-11-28 | Max phase material, preparation method therefor and application thereof |
| PCT/CN2018/117811 WO2020010783A1 (en) | 2018-07-10 | 2018-11-28 | Max phase material, preparation method therefor, and application thereof |
| EP18926353.6A EP3778479B1 (en) | 2018-07-10 | 2018-11-28 | Max phase material, preparation method therefor, and application thereof |
| JP2020546500A JP7030362B2 (en) | 2018-07-10 | 2018-11-28 | MAX phase material, its preparation method and use |
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| CN109437177A (en) * | 2018-12-04 | 2019-03-08 | 中国科学院宁波材料技术与工程研究所 | Using Cl as MXene material of surface group and the preparation method and application thereof |
| CN110668821A (en) * | 2019-11-12 | 2020-01-10 | 中国工程物理研究院核物理与化学研究所 | Method for preparing MAX phase ceramic under no pressure |
| WO2020114196A1 (en) * | 2018-12-04 | 2020-06-11 | 中国科学院宁波材料技术与工程研究所 | Mxene material, preparation method therefor and application thereof |
| CN111393167A (en) * | 2020-03-25 | 2020-07-10 | 宁波材料所杭州湾研究院 | Novel MAX phase composite material and preparation method thereof |
| CN111725380A (en) * | 2020-06-12 | 2020-09-29 | 清华大学 | Layered high-entropy MAX-phase ceramic thermoelectric material and preparation method thereof |
| CN111943205A (en) * | 2020-08-28 | 2020-11-17 | 郑州轻工业大学 | Method for preparing MAX phase by adopting melt displacement reaction, prepared MAX phase and application |
| CN112938977A (en) * | 2021-03-31 | 2021-06-11 | 中国科学院宁波材料技术与工程研究所 | MAX phase material with A site as noble metal element, preparation method and application thereof |
| CN113816378A (en) * | 2021-11-11 | 2021-12-21 | 中国科学院宁波材料技术与工程研究所 | MAX phase layered material containing antimony element at A position, preparation method and application thereof |
| CN114853013A (en) * | 2021-02-04 | 2022-08-05 | 中国科学院宁波材料技术与工程研究所 | Novel ternary layered rare earth MAX phase material and preparation method and application thereof |
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