CN115594181A - Aluminum-excess MAX phase ceramic and preparation method thereof - Google Patents
Aluminum-excess MAX phase ceramic and preparation method thereof Download PDFInfo
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- CN115594181A CN115594181A CN202110772522.3A CN202110772522A CN115594181A CN 115594181 A CN115594181 A CN 115594181A CN 202110772522 A CN202110772522 A CN 202110772522A CN 115594181 A CN115594181 A CN 115594181A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 4
- 229910019637 Nb2AlC Inorganic materials 0.000 claims abstract 4
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract 3
- 239000000843 powder Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims 1
- 238000003828 vacuum filtration Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 15
- 239000000203 mixture Substances 0.000 description 9
- 229910018575 Al—Ti Inorganic materials 0.000 description 7
- 238000005245 sintering Methods 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses an aluminum excess MAX phase ceramic and a preparation method thereof, relates to Nb2AlC, V2AlC and Ti2AlC phase ceramic, and belongs to the technical field of nano materials. The material is prepared by adjusting Nb: al: nbC or V: al: c or TiH2: al: and grinding the TiC by a ball mill, calcining, washing, filtering, drying and screening to prepare the MAX phase ceramic with excessive aluminum.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to an aluminum excess MAX phase ceramic and a preparation method thereof.
Background
The MAX phase ceramic is a precursor for preparing a two-dimensional MXene material, and with the continuous and intensive research on MXene, researchers continuously explore a new synthesis route and a new processing method for improving the quality of MXene. At present, most methods mainly focus on post-treatment and post-storage, such as nitrogen introduction, treatment under vacuum condition, low-temperature storage and organic solvent storage. Few studies have placed the center of gravity of the work on the precursor preparation process. In recent years, some methods of making MAX phase ceramics have simply changed the composition of the raw materials. Such as Ti 3 AlC 2 The phase ceramic is prepared by the combination of Ti/Al/C, ti/Al/TiC and Ti/Al/C/TiC at first, the raw material combination uses metallic titanium powder as a titanium source, and the titanium powder is expensive, thereby causing Ti to be generated 3 AlC 2 High cost of (2). In order to make the cost controllable, researchers have adopted TiH 2 /Al/TiC,TiH 2 Sintering of Ti with combination of/Al/C 3 AlC 2 Phase ceramics, tiH 2 The powder is an intermediate product for the manufacture of metallic Ti powder and is cheaper than Ti powder. In addition to this cost-saving effect,the quality performance of MXene is not improved at all. Recently, yury Gogotsi is entitled "Modified MAX Phase Synthesis for environmental Stable and Highlyconductive Ti 3 C 2 MXene article reports preparation of antioxidant two-dimensional Ti 3 C 2 A new method for MXene material.
In view of this, the present invention proposes that by adjusting the molar ratio for the preparation of MAX phase ceramics, an excess of aluminium will result in M with improved stoichiometry and crystallinity n+1 AlX n The quality of the prepared MXene material is improved and the performance is improved due to the generation of crystal grains. Provides a new idea and thought for solving the problem of easy oxidation of MXene materials.
Disclosure of Invention
In order to improve the quality and performance of the MXene material, the invention starts from MAX phase precursors and aims to provide an aluminum excess MAX phase ceramic and a preparation method thereof. The invention adopts NbC/Nb/Al, V/Al/C and TiH 2 Taking Al/TiC as a raw material, grinding by a ball mill, calcining, washing, filtering, drying and screening to finally obtain Al-excessive Nb 2 AlC、V 2 AlC、Ti 2 And (4) AlC. The difference from the traditional preparation method is that: during the preparation of the MAX phase, excess aluminum is added, and ball-milled and mixed uniformly. The presence of molten metal during the sintering reaction promotes the diffusion of the reactants, resulting in Nb 2 AlC、V 2 AlC、Ti 2 The AlC grains have improved structural order and morphology. Then subjecting the Al-Nb to 2 AlC、Al-V 2 AlC、Al-Ti 2 AlC for synthesizing high-quality Nb 2 CT x 、V 2 CT x 、Ti 2 CT x Nanosheets. The MXene material prepared by the method for preparing the MAX-phase ceramic with excessive aluminum has higher conductivity and stronger oxidation resistance, and the shelf life of MXene solution is prolonged.
The technical scheme of the invention comprises the following steps:
step 1: taking NbC: nb: xAl (x)>1, ensuring excessive Al addition) to produce Nb 2 Powder of AlC; and (3) adding the following components in a volume of 2V: xAl: c (x)>1, ensuring excessive Al addition) are mixed in a molar ratioCo-production of V 2 Powder of AlC; selecting 2TiH 2 : xAl: c and TiH 2 :xAl:TiC(x>1, ensuring excessive Al to be added) as a raw material to synthesize Ti2AlC;
and 2, step: grinding the powders by a ball mill for 12-18h at the rotating speed of 60-100 rpm to ensure that the raw materials are uniformly mixed, and then putting the mixture into a corundum crucible;
and step 3: calcining the sample in a tube furnace at 1300-1700 ℃ for 90-150 minutes under the argon atmosphere at the heating rate of 5-15 ℃/min to obtain Al-Nb 2 AlC、Al-V 2 AlC、Al-Ti 2 Sintering AlC blocks;
and 4, step 4: soaking in 6-12M HCl for not less than 4 hr to remove excess metallic Al until Al-Nb 2 AlC、Al-V 2 AlC、Al-Ti 2 No bubble escapes from the AlC phase ceramic solution;
and 5: respectively filtering Al-Nb by using filter membranes with the aperture of 0.45 mu m 2 AlC/HCl、Al-V 2 AlC/HCl、Al-Ti 2 Repeatedly filtering the AlC/HCl mixture by using deionized water until the mixture is nearly neutral;
and 6: then drying the MAX phase ceramic with excessive aluminum in a vacuum oven at 60 to 80 ℃ for at least 6 h;
and 7: and finally, classifying and screening through a particle sieve of 400 or 800 meshes, and storing for later use.
Preferably, the rotation speed of the ball mill is 80 rpm, and the grinding time is 18 h;
preferably, the calcination temperature is 1400 ℃, the calcination time is 120 minutes, the heating rate is 10 ℃/min, and the atmosphere is argon;
preferably, the 9M HCl soak is performed for 12 h, repeated three times.
Compared with the prior art, the invention has the following beneficial effects:
(1) Al-excess prepared Nb 2 AlC、V 2 AlC、Ti 2 The AlC crystal grains have improved structural order and morphology, and produce MAX phase with improved structure and maximum stoichiometric ratio, and the obtained MXene is improved;
(2) The MXene material flakes prepared from the MAX phase ceramic with excess aluminum have improved quality and higher electronic conductivity;
(3) The prepared MXene has better oxidation resistance, thereby obviously improving the storage life and the chemical stability of the MXene and providing simplicity for the research of the MXene.
Drawings
FIG. 1 shows Al excess Nb 2 XRD pattern of AlC;
FIG. 2 shows the Al excess Nb 2 SEM image of AlC;
FIG. 3 shows the Al excess Nb 2 TEM image of AlC.
Detailed Description
The essence of the invention is described in detail below with reference to the following examples:
example 1
In the present example, al-Nb was produced by the following method 2 AlC:
With NbC: nb:1.2 molar ratio of Al to mix and produce Al-excess Nb 2 Powders of AlC; these powders were milled for 18h by a ball mill at 80 rpm to ensure uniform mixing of the raw materials and placed in a corundum crucible. Calcining the sample in a tube furnace at 1650 ℃ for 90 minutes in argon gas atmosphere at the heating rate of 15 ℃/min to obtain Al-Nb 2 AlC、Al-V 2 AlC、Al-Ti 2 And sintering AlC blocks. Soaking for 6 h by using 9M HCl, and repeating for three times to remove excessive metal Al until no more bubbles escape from the Al-MALX phase solution; vacuum filtering Al-Nb with filter membrane with pore diameter of 0.45 μm 2 Repeatedly filtering the AlC/HCl mixture by using deionized water, washing to be neutral, and drying for 6 h in a vacuum oven at 60 ℃. Then drying the Al-Nb 2 Sieving the AlC through a 400-mesh particle sieve;
example 2
In this example, V was prepared by the following method 2 AlC:
And (3) adding the following components in a volume of 2V:1.2Al: production of aluminum excess V by mixing C molar ratio 2 Powder of AlC; these powders were milled for 12 h by a ball mill at 80 rpm to ensure uniform mixing of the raw materials and placed in a corundum crucible. Calcining the sample in a tube furnace at 1450 ℃ for 120 minutes in argon gas atmosphere at a heating rate of 10 ℃/min to obtain Al-V 2 And sintering AlC blocks. Soaking with 9M HCl for 12 hr, and repeatingTwice to remove excess metallic Al until Al-V 2 No more bubbles escape from the AlC phase solution; vacuum filtering Al-V with filter membrane with pore diameter of 0.45 μm 2 Repeatedly filtering the AlC/HCl mixture by using deionized water, washing to be neutral, and drying for 6 h in a vacuum oven at 60 ℃. Then drying the Al-Nb 2 Sieving AlC through a 400-mesh particle sieve;
example 3
In the present example, ti was prepared by the following method 2 AlC MXene:
And (3) adding the following components in a volume of 2V:1.2Al: mixing of molar ratio of C to produce Ti with excess aluminum 2 Powder of AlC; these powders were milled for 18h by a ball mill at 60 rpm to ensure uniform mixing of the raw materials and placed in a corundum crucible. Calcining the sample in a tube furnace at 1500 ℃ for 120 minutes in argon gas atmosphere at a heating rate of 10 ℃/min to obtain Al-V 2 And sintering AlC blocks. Soaking for 12 h by using 9M HCl, and repeating twice to remove excessive metal Al until no bubbles escape from the Al-MALX phase solution; vacuum filtering Al-Ti with filter membrane with pore diameter of 0.45 mu m 2 Repeatedly filtering the AlC/HCl mixture by using deionized water, washing the mixture to be neutral, and drying the mixture for 6 hours in a vacuum oven at 60 ℃. Then drying the Al-Ti 2 The AlC was sieved through a 400 mesh particle sieve.
The above contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention should not be limited thereby, and any modification made on the basis of the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. The MAX phase ceramic is characterized by comprising Nb2AlC, V2AlC and Ti2AlC, the preparation method takes Nb, al, nbC, V, C, tiH2 and TiC as raw materials, and the aluminum excess means that the aluminum added in the MAX phase ceramic preparation process is excessive.
2. The improved MAX phase precursor for excess aluminum and method of making the same as claimed in claim 1 comprising the steps of: grinding the powder of the NbC/Nb/Al combination or V/Al/C combination or TiH2/Al/TiC combination by a ball mill, calcining, washing, filtering, drying and screening to finally obtain Nb2AlC, V2AlC and Ti2AlC with excessive Al.
3. The method of claim 2, wherein the ratio of NbC: nb: mixing the molar ratio of xAl to prepare Nb2AlC powder; 2V: xAl: c, mixing the prepared V2AlC powder according to the molar ratio; selected from the group consisting of TiH2: xAl: the molar ratio of TiC is used as raw material to mix and prepare Ti2AlC, wherein x is more than 1, and the excessive addition of Al is ensured.
4. The method of claim 2, wherein the ball milling is performed at 60-100 rpm for 12-18h.
5. The method according to claim 2, wherein the calcination temperature is 1300-1700 ℃, the calcination time is 90-150 minutes, the heating rate is 5-15 ℃/min, and the atmosphere is argon.
6. The method of claim 2, wherein the washing is with HCl at a concentration of 6-12M for a time of not less than 4 h.
7. The method as claimed in claim 2, wherein the filtration is vacuum filtration using a filter membrane with a pore size of 0.45 μm, and repeated washing is performed until the solution is neutral.
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CN1884064A (en) * | 2006-07-12 | 2006-12-27 | 中国科学院上海硅酸盐研究所 | Method for preparing Cr2AlC by molten salt process |
CN107257866A (en) * | 2015-02-09 | 2017-10-17 | 法国国家航空航天研究院 | The method of cermet material and this material of manufacture |
CN108341670A (en) * | 2018-02-02 | 2018-07-31 | 西南科技大学 | Single-phase Ti3SiC2The preparation method of cermet |
CN108821291A (en) * | 2018-07-10 | 2018-11-16 | 中国科学院宁波材料技术与工程研究所 | A kind of novel tertiary stratiform MAX phase material, preparation method and application |
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 |
CN112316157A (en) * | 2020-11-12 | 2021-02-05 | 苏州北科纳米科技有限公司 | Preparation method and application of antioxidant MXenes material |
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- 2021-07-08 CN CN202110772522.3A patent/CN115594181A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1884064A (en) * | 2006-07-12 | 2006-12-27 | 中国科学院上海硅酸盐研究所 | Method for preparing Cr2AlC by molten salt process |
CN107257866A (en) * | 2015-02-09 | 2017-10-17 | 法国国家航空航天研究院 | The method of cermet material and this material of manufacture |
CN108341670A (en) * | 2018-02-02 | 2018-07-31 | 西南科技大学 | Single-phase Ti3SiC2The preparation method of cermet |
CN108821291A (en) * | 2018-07-10 | 2018-11-16 | 中国科学院宁波材料技术与工程研究所 | A kind of novel tertiary stratiform MAX phase material, preparation method and application |
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 |
CN112316157A (en) * | 2020-11-12 | 2021-02-05 | 苏州北科纳米科技有限公司 | Preparation method and application of antioxidant MXenes material |
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