CN109592684A - A kind of petal spherical carbide titanium and its preparation method and application - Google Patents
A kind of petal spherical carbide titanium and its preparation method and application Download PDFInfo
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- CN109592684A CN109592684A CN201811546933.5A CN201811546933A CN109592684A CN 109592684 A CN109592684 A CN 109592684A CN 201811546933 A CN201811546933 A CN 201811546933A CN 109592684 A CN109592684 A CN 109592684A
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- titanium
- petal
- spherical carbide
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- 239000010936 titanium Substances 0.000 title claims abstract description 93
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 31
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 43
- 239000000843 powder Substances 0.000 claims description 42
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 33
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 24
- 239000000138 intercalating agent Substances 0.000 claims description 21
- 238000002604 ultrasonography Methods 0.000 claims description 19
- 238000005530 etching Methods 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 13
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 6
- 229910001416 lithium ion Inorganic materials 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- 239000010436 fluorite Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 33
- 239000000126 substance Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 66
- 235000019441 ethanol Nutrition 0.000 description 34
- 229960004756 ethanol Drugs 0.000 description 21
- 238000005406 washing Methods 0.000 description 21
- 239000011343 solid material Substances 0.000 description 19
- 238000000498 ball milling Methods 0.000 description 17
- 229910009819 Ti3C2 Inorganic materials 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- 239000000725 suspension Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 9
- 229960000935 dehydrated alcohol Drugs 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910021642 ultra pure water Inorganic materials 0.000 description 5
- 239000012498 ultrapure water Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910021397 glassy carbon Inorganic materials 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000013065 commercial product Substances 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 239000012621 metal-organic framework Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052757 nitrogen Chemical group 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 description 1
- MERJTCXDDLWWSK-UHFFFAOYSA-N 1-methylpyrrole pyrrolidin-2-one Chemical compound CN1C=CC=C1.N1C(CCC1)=O MERJTCXDDLWWSK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000219289 Silene Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- -1 antimony alkene Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013310 covalent-organic framework Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C01P2004/32—Spheres
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Abstract
The invention belongs to technical field of material, and in particular to a kind of petal spherical carbide titanium and its preparation method and application.Petal spherical carbide titanium provided by the invention, by being constituted with a thickness of the nanometer sheet of 20~30nm；The petal spherical carbide titanium has hole, and the aperture of hole is 20~50nm；The partial size of the petal spherical carbide titanium is 200~300nm.Titanium carbide provided by the invention constitutes petal spherical structure by ultrathin nanometer piece, so that titanium carbide is had excellent nano effect and biggish specific surface area, improves the chemical property of material.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of petal spherical carbide titanium and preparation method thereof and answer
With.
Background technique
After Novoselov and Geim in 2004 and its partner successfully separate graphene, the research of two-dimensional material
Enter the period of high speed development.At the same time, class grapheme material is also greatly enriched two-dimensional material family, such as two dimension
Transition metal carbide or carbonitride (MXenes), black phosphorus, metal-organic framework material (MOFs), covalent organic frame material
(COFs), polymer, silene, antimony alkene, inorganic perovskite and organic and inorganic mixing perovskite etc. occur in succession.
MXenes is a kind of two-dimensional layer transition metal carbide or nitride, such compound are by the way that MAX phase exists
Selective etch removes neutral element and a kind of New Two Dimensional material for generating in hydrofluoric acid solution, and wherein M is Ti, Mo, Sc, Zr
Equal transition metal elements, A are major element (mostly Al, Si), and X is carbon or nitrogen.MXenes material is based on its unique stratiform knot
Structure, excellent metallic conductivity, hydrophily, chemical property and big specific surface area obtain extensively in hydrogen storage and electrochemical field
General application, for example, Ti3C2Mxene material is just led in hydrogen storage, lithium ion battery, electro-catalysis, supercapacitor and sensor etc.
Domain shows the application prospect of great potential.Currently used Ti3C2Although Mxene material has the characteristics that stratiform, as electrification
When learning materials'use, metallic conduction performance is unsatisfactory, limits the application of such material.
Summary of the invention
It is provided by the invention the purpose of the present invention is to provide a kind of petal spherical carbide titanium and its preparation method and application
Titanium carbide has petal spherical structure, and large specific surface area has excellent chemical property.
To achieve the goals above, the invention provides the following technical scheme:
The present invention provides a kind of petal spherical carbide titaniums, by constituting with a thickness of the nanometer sheet of 20~30nm；The petal
Spherical carbide titanium has hole, and the aperture of hole is 20~50nm；The partial size of the petal spherical carbide titanium is 200~300nm.
Preferably, the specific surface area of the petal spherical carbide titanium is 28~40m2·g-1。
The present invention provides the preparation methods of petal spherical carbide titanium described in above-mentioned technical proposal, comprising the following steps:
(1) under agitation, by Ti3AlC2Powder is added in hydrofluoric acid solution, and titanium carbide is obtained after etching；
(2) it under ultrasound condition, is removed, is obtained using the titanium carbide that different intercalators obtains the step (1)
To petal spherical carbide titanium；
The intercalator includes N,N-dimethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide or acetonitrile.
Preferably, Ti in the step (1)3AlC2The partial size of powder≤300 mesh.
Preferably, the mass concentration of hydrofluoric acid solution is 10~30% in the step (1).
Preferably, Ti in the step (1)3AlC2The quality of powder and volume ratio >=1g:10mL of hydrofluoric acid solution.
Preferably, Ti in the step (1)3AlC2The adding speed of powder is 0.1~0.5g/min.
Preferably, the time etched in the step (1) is 24~48h.
Preferably, power ultrasonic in the step (2) is 180~240W；Ultrasound time be 8~for 24 hours.
The present invention also provides described in above-mentioned technical proposal petal spherical carbide titanium or above-mentioned technical proposal described in make
The petal spherical carbide titanium that Preparation Method is prepared is in hydrogen storage, lithium ion battery, electro-catalysis, supercapacitor or sensor field
Application.
Petal spherical carbide titanium provided by the invention, by being constituted with a thickness of the nanometer sheet of 20~30nm；The petal is spherical
Titanium carbide has hole, and the aperture of hole is 20~50nm；The partial size of the petal spherical carbide titanium is 200~300nm.This hair
The titanium carbide of bright offer constitutes petal spherical structure by ultrathin nanometer piece, and titanium carbide is made to have excellent nano effect and biggish
Specific surface area improves the chemical property of material.
Petal spherical carbide titanium provided by the invention is removed respectively using different intercalators and is obtained under ultrasonic wave added,
Method is simple and easy to control, low in cost.
Petal spherical carbide titanium material provided by the invention has excellent electric conductivity, urges in hydrogen storage, lithium ion battery, electricity
Change, supercapacitor and sensor field have application value.
Detailed description of the invention
Fig. 1 is the titanium carbide scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 obtains；
Fig. 2 is the scanning electron microscope (SEM) photograph for the petal spherical carbide titanium that the embodiment of the present invention 1 obtains；
Fig. 3 is the transmission electron microscope picture for the petal spherical carbide titanium that the embodiment of the present invention 2 obtains；
Fig. 4 is the X-ray diffractogram for the petal spherical carbide titanium that the embodiment of the present invention 3 obtains；
Fig. 5 is the ac impedance measurement figure for the petal spherical carbide titanium modified glassy carbon electrode that the embodiment of the present invention 3 obtains；
Fig. 6 is the pictorial diagram for the petal spherical carbide titanium dispersion liquid that the embodiment of the present invention 4 obtains.
Specific embodiment
The present invention provides a kind of petal spherical carbide titaniums, by constituting with a thickness of the nanometer sheet of 20~30nm；The petal
Spherical carbide titanium has hole, and the aperture of hole is 20~50nm；The partial size of the petal spherical carbide titanium is 200~300nm.
Petal spherical carbide titanium provided by the invention with a thickness of the nanometer sheet of 20~30nm by constituting, the thickness of the nanometer sheet
Degree is preferably 20~28nm, more preferably 20~25nm；The petal spherical carbide titanium has a hole, and the aperture of hole is 20~
50nm, preferably 30~50nm；The partial size of the petal spherical carbide titanium be 200~300nm, preferably 210~280nm, more
Preferably 220~270nm.In the present invention, the nanometer sheet in petal spherical carbide titanium forms hole because being in irregular alignment
Structure, and then increase the specific surface area of petal spherical carbide titanium.In the present invention, the specific surface of the petal spherical carbide titanium
Product is preferably 28~40m2·g-1, more preferably 32~40m2·g-1。
The present invention provides the preparation methods of petal spherical carbide titanium described in above-mentioned technical proposal, comprising the following steps:
(1) under agitation, by Ti3AlC2Powder is added in hydrofluoric acid solution, and titanium carbide is obtained after etching；
(2) it under ultrasound condition, is removed, is obtained using the titanium carbide that different intercalators obtains the step (1)
To petal spherical carbide titanium；
The intercalator includes N,N-dimethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide or acetonitrile.
The present invention under agitation, by Ti3AlC2Powder is added in hydrofluoric acid solution, and titanium carbide is obtained after etching.
In the present invention, the Ti3AlC2The partial size of powder preferably≤300 mesh, more preferably 350~500 mesh.The present invention couple
The Ti3AlC2The source of powder does not have particular/special requirement, uses commercial product well known to those skilled in the art.The present invention is excellent
Choosing is to commercially available Ti3AlC2Powder carries out ball milling, so that Ti3AlC2The uniform particle sizesization of powder.In the present invention, to commercially available
Ti3AlC2When powder carries out ball milling, preferably wet-milling, wet-milling agents useful for same is preferably ethyl alcohol；When ball milling, commercially available Ti3AlC2Powder
Quality and the volume ratio of ethyl alcohol are preferably (5~10) g:(30~50) mL, more preferably (6~9) g:(35~45) mL；Revolving speed is excellent
It is selected as 300~450r/min, more preferably 320~430r/min；Ball-milling Time is preferably 2~4h, more preferably 2.5~
3.5h.The present invention is preferably to Ti3AlC2Powder carries out ball milling, can make the granularity refinement and homogenization of powder, shorten subsequent titanium carbide
Preparation time, moreover it is possible to improve the electric property of titanium carbide material to a certain extent.
After ball milling, the present invention preferably washs the slurry after ball milling with ethyl alcohol, and washing times are preferably 3~6 times；It washes
After washing, the present invention is preferably dried the solid material after washing, and the temperature of the drying is preferably 50~80 DEG C, more preferably
55~75 DEG C；The dry time is preferably 12~for 24 hours, more preferably 14~20h.After drying, the present invention preferably will be after drying
Material is sieved, and screenings is required Ti3AlC2Powder.The present invention does not have special want to the mesh number of the sieving sieve
It asks, the Ti of above-mentioned partial size can be obtained3AlC2Powder.
In the present invention, the Ti3AlC2Powder is added in hydrofluoric acid solution under agitation, the speed of the stirring
Preferably 200~500r/min, more preferably 250~450r/min are further preferably 300~400r/min；The speed of addition is excellent
It is selected as 0.1~0.5g/min, more preferably 0.13~0.47g/min, is further preferably 0.15~0.45g/min.
In the present invention, the mass concentration of the hydrofluoric acid solution is preferably 10~30%, and more preferably 12~28%, then
Preferably 15~25%.The present invention does not have particular/special requirement to the source of the hydrofluoric acid, and use is well known to those skilled in the art
Commercial product.In the present invention, when etching, the Ti3AlC2The quality of powder and the volume ratio of hydrofluoric acid solution preferably >=
1g:10mL, more preferably (1~5) g:10mL are further preferably (1.5~4.5) g:10mL.In the present invention, the time of etching from
Ti3AlC2It is counted after the completion of powder addition, the time of the etching is preferably 24~48h, more preferably 26~45h, further preferably for 28~
42h；In the present invention, etching process auxiliary is to stir, and the speed of the stirring is preferably 200~500r/min, more preferably
250~450r/min is further preferably 300~400r/min.
In the present invention, the etching refers to hydrofluoric acid and Ti3AlC2Al reaction in powder, generates the process of titanium carbide.This hair
It is bright preferably to etch under the above conditions, it had both been avoided that titanium carbide dissolved, and had improved the yield of titanium carbide, moreover it is possible to eliminate lacking for titanium carbide
It falls into, and then obtains the higher titanium carbide of electric conductivity.
After etching, the present invention preferably washs the black solid material obtained after etching, to remove remaining hydrogen fluorine
Acid obtains pure titanium carbide.In the present invention, the washing is preferably ultrapure water with reagent.The present invention is to the washing
Mode does not have particular/special requirement, and the pH value of cleaning solution is preferably made to reach 5~6.
After obtaining titanium carbide, the present invention removes the titanium carbide under ultrasound condition, using different intercalators,
Obtain petal spherical carbide titanium.In the present invention, the intercalator includes n,N-Dimethylformamide (DMF), N- methylpyrrole
Alkanone (NMP), dimethyl sulfoxide (DMSO) or acetonitrile, more preferably n,N-Dimethylformamide, N-Methyl pyrrolidone or
Dimethyl sulfoxide.
In the present invention, the different intercalator preferably includes two different intercalators.When the different intercalation
When agent is two different intercalators, the present invention such as gives a definition to stripping process: removing is divided into the first time successively carried out
Removing and second of removing, the intercalator of removing for the first time is the first intercalator；Second of removing intercalator is the second intercalation
Agent.
In the present invention, when first intercalator is n,N-Dimethylformamide, the second intercalator is preferably N- methyl
Pyrrolidones, dimethyl sulfoxide or acetonitrile, more preferably N-Methyl pyrrolidone or dimethyl sulfoxide；
When first intercalator is N-Methyl pyrrolidone, second intercalator is preferably N, N- dimethyl formyl
Amine, dimethyl sulfoxide or acetonitrile, more preferably n,N-Dimethylformamide or dimethyl sulfoxide；
When first intercalator is dimethyl sulfoxide, second intercalator is preferably n,N-Dimethylformamide, N-
Methyl pyrrolidone or acetonitrile, more preferably n,N-Dimethylformamide or N-Methyl pyrrolidone；
When first intercalator is acetonitrile, second intercalator is preferably n,N-Dimethylformamide, N- methyl pyrrole
Pyrrolidone or dimethyl sulfoxide, more preferably n,N-Dimethylformamide or dimethyl sulfoxide.
In the present invention, when the intercalator is two different intercalators, the body of the first intercalator and the second intercalator
Product is than being 0.8~1.5:1, more preferably 0.9~1.3:1.
In the present invention, when removing for the first time, the volume ratio of the quality of titanium carbide and the first intercalator be preferably (0.5~
1.2) g:15mL, more preferably (0.6~1.1) g:15mL are further preferably (0.6~1.0) g:15mL；Ultrasound power be preferably
180~240W, more preferably 200~220W；The time of ultrasound is preferably 8~for 24 hours, more preferably 8~22h is further preferably 10
~16h；The time of the ultrasound is the time of removing for the first time.
It completes after removing for the first time, the upper layer suspension after the present invention preferably removes first time is centrifuged, by gained
Solid material alcohol carries out second after washing and removes.In the present invention, the revolving speed of the centrifugation is preferably 5000~8000r/min；Institute
Stating alcohol and washing with detergent is preferably ethyl alcohol；The number that the alcohol is washed is preferably 3~6 times.The present invention washes the alcohol specific clear
The mode of washing does not have particular/special requirement, using well known to those skilled in the art.After alcohol is washed, the present invention is preferably to last time alcohol
Dispersion liquid when washing is centrifuged, and the solid after removing for the first time is obtained.
In the present invention, when second of removing, the volume ratio of solid masses and the second intercalator after removing for the first time is excellent
It is selected as (0.37~0.75) g:15mL, more preferably (0.45~0.75) g:15mL, is further preferably (0.45~0.6) g:15mL；
The power of ultrasound is preferably 180~240W, more preferably 200~220W；The time of ultrasound is preferably 8~for 24 hours, more preferably 8
~22h is further preferably 10~16h；The time of the ultrasound is the time of second of removing.
In the present invention, in etch step, first time strip step and second of strip step, titanium carbide can generate can not
The loss avoided, therefore, second of removing solid masses can be less than the quality for removing solid for the first time.
It completes second after removing, gained upper layer suspension is centrifuged after the present invention will preferably remove for second, then
Obtained solid material progress alcohol is washed.In the present invention, the revolving speed of the centrifugation is preferably 5000~8000r/min；The alcohol is washed
It is preferably ethyl alcohol with detergent；The number that the alcohol is washed is preferably 2~4 times, and more preferably 3 times；After alcohol is washed, the present invention is preferably right
Alcohol is washed rear obtained solid material and is dried, and petal spherical carbide titanium is obtained.The present invention does not have special want to the mode of the drying
It asks, the alcohol in solid material can be removed and washed with detergent.
The present invention also provides described in above-mentioned technical proposal petal spherical carbide titanium or above-mentioned technical proposal described in make
The petal spherical carbide titanium that Preparation Method is prepared is in hydrogen storage, lithium ion battery, electro-catalysis, supercapacitor and sensor field
Application.Concrete application mode of the present invention to the petal spherical carbide titanium in above-mentioned field does not have particular/special requirement, using this
Mode known to the technical staff of field.
In order to further illustrate the present invention, with reference to the accompanying drawings and examples to a kind of petal spherical shape carbon provided by the invention
Change titanium and its preparation method and application to be described in detail, but they cannot be interpreted as to the limit to the scope of the present invention
It is fixed.
Embodiment 1
Firstly, the Ti that 5g is bought3AlC2Stock dispersion is into the ball grinder equipped with 30mL ethanol reagent, with 350r/min
Revolving speed ball milling 2h, obtain uniform slurry.Then, using dehydrated alcohol filtration washing slurry 3 times, and 50 in vacuum drying oven
Dry 12h at DEG C, by the Ti after ball milling3AlC2Powder, be placed in the sieve of 300 mesh sieve partial size less than 300 mesh Ti3AlC2
Powder.At room temperature, the hydrofluoric acid solution that mass fraction is 10% is poured into plastic containers, is put into rotor, by magnetic agitation speed
Degree is adjusted to 200r/min, the Ti after 2g ball milling is then slowly added into 10min3AlC2Powder, stirring while adding, wherein 1g
Ti3AlC2Powder corresponds to 10mL hf etching solution, keeps magnetic agitation for 24 hours.Next, by above-mentioned mixed liquor in ultrapure water
Middle eccentric cleaning to supernatant pH value is 5~6.Finally, after obtained black precipitate is washed 3 times with DMF solvent, will
To solid material first in the DMSO of 15mL with 200W ultrasonic power ultrasound 8h, take upper layer suspension to be centrifuged, gained consolidated
Body material is with after ethyl alcohol centrifuge washing 3 times, by obtained solid material again in DMF with 200W ultrasonic power ultrasound 8h, DMSO and DMF
Dosage volume ratio be 1:1, take upper layer suspension to be centrifuged, will be dry after obtained solid material ethyl alcohol centrifuge washing 3 times,
Petal spherical shape Ti can be obtained3C2The solid of Mxene material.
Embodiment 2
Firstly, the Ti that 5g is bought3AlC2Stock dispersion is into the ball grinder equipped with 50mL ethanol reagent, with 400r/min
Revolving speed ball milling 3h, obtain uniform slurry.Then, using dehydrated alcohol filtration washing slurry 3 times, and 80 in vacuum drying oven
Dry 12h at DEG C, by the Ti after ball milling3AlC2Powder, be placed in the sieve of 300 mesh sieve partial size less than 300 mesh Ti3AlC2
Powder.At room temperature, the hydrofluoric acid solution that mass fraction is 20% is poured into plastic containers, is put into rotor, by magnetic agitation speed
Degree is adjusted to 250r/min, the Ti after 3g ball milling is then slowly added into 15min3AlC2Powder, stirring while adding, wherein 1g
Ti3AlC2Powder corresponds to 10mL hf etching solution, keeps magnetic agitation 36h.Next, by above-mentioned mixed liquor in ultrapure water
Middle eccentric cleaning to supernatant pH value is 5~6.Finally, after obtained black precipitate is washed 3 times with dehydrated alcohol, it will
Obtained solid material takes upper layer suspension to be centrifuged, by gained first in the NMP of 15mL with 200W ultrasonic power ultrasound 10h
Solid material is ultrasonic again with 200W ultrasonic power in the DMSO of 12mL by obtained solid material with after ethyl alcohol centrifuge washing 4 times
10h takes upper layer suspension to be centrifuged, and obtained solid material is dry later with ethyl alcohol centrifuge washing 3 times, and petal ball can be obtained
Shape Ti3C2The solid of Mxene material.
Embodiment 3
Firstly, the Ti that 8g is bought3AlC2Powder is distributed in the ball grinder equipped with 50mL ethanol reagent, with 450r/min
Revolving speed ball milling 4h, obtain uniform slurry.Then, using dehydrated alcohol filtration washing slurry 5 times, and 80 in vacuum drying oven
Dry 16h at DEG C, and the Ti that will be obtained3AlC2Powder, be placed in the sieve of 300 mesh sieve partial size less than 300 mesh Ti3AlC2
Powder.At room temperature, the hydrofluoric acid solution that mass fraction is 10% is poured into plastic containers, is put into rotor, by magnetic agitation speed
Degree is adjusted to 300r/min, the Ti after 3g ball milling is then slowly added into 10min3AlC2Powder, stirring while adding, wherein 1g
Ti3AlC2Powder corresponds to 10mL hf etching solution, keeps magnetic agitation for 24 hours.Next, by above-mentioned mixed liquor in ultrapure water
Middle eccentric cleaning to supernatant pH be 5~6.Finally, will be obtained after obtained black precipitate is washed 3 times with nmp solvent
Solid material first in the DMF of 12mL with 200W ultrasonic power ultrasound for 24 hours, take upper layer suspension to be centrifuged, by obtained solid
After material is used ethyl alcohol centrifuge washing 5 times, by obtained solid material, with 200W ultrasonic power, ultrasound for 24 hours, is taken again in the NMP of 15mL
Layer suspension is centrifuged, and obtained solid material is dry later with ethyl alcohol centrifuge washing 3 times, and petal spherical shape can be obtained
Ti3C2The solid of Mxene material.
Embodiment 4
Firstly, the Ti that 10g is bought3AlC2Powder is distributed in the ball grinder equipped with 30mL ethanol reagent, with 450r/min
Revolving speed ball milling 4h, obtain uniform slurry.Then, using dehydrated alcohol filtration washing slurry 3 times, and 80 in vacuum drying oven
It is dried for 24 hours at DEG C, and the Ti that will be obtained3AlC2Powder, be placed in the sieve of 300 mesh sieve partial size less than 300 mesh Ti3AlC2
Powder.At room temperature, the hydrofluoric acid solution that mass fraction is 30% is poured into plastic containers, is put into rotor, by magnetic agitation speed
Degree is adjusted to 500r/min, the Ti after 5g ball milling is then slowly added into 15min3AlC2Powder, stirring while adding, wherein 1g
Ti3AlC2Powder corresponds to 10mL hf etching solution, keeps magnetic agitation 48h.Next, by above-mentioned mixed liquor in ultrapure water
Middle eccentric cleaning to pH value reaches 6 or so.Finally, after obtained black precipitate is washed 3 times with dehydrated alcohol, in the second of 30mL
With 200W ultrasonic power ultrasound 16h in nitrile, upper layer suspension is taken to be centrifuged, by obtained solid material with ethyl alcohol centrifuge washing 6 times
Later, by obtained solid material in the DMSO of 35mL with 200W ultrasonic power ultrasound 16h again, take upper layer suspension to be centrifuged,
Obtained solid material is dry later with ethyl alcohol centrifuge washing 3 times, petal spherical shape Ti can be obtained3C2The solid of Mxene material.
Performance characterization and result
It is characterized using pattern of the scanning electron microscope to titanium carbide obtained by Examples 1 to 4 and petal spherical carbide titanium.Fig. 1
For the titanium carbide that embodiment 1 is prepared, 1 gained titanium carbide of embodiment is the layer structure of similar " accordion " as shown in Figure 1,
The thickness of the structure is about 200~300nm.Fig. 2 is the petal spherical carbide titanium that embodiment 1 is prepared, as shown in Figure 2, flower
Valve spherical carbide titanium can provide big active surface area and activity abundant by constituting with a thickness of the nanometer sheet of 20~30nm
Site.2~4 test result of embodiment is close with embodiment 1, is petal spherical carbide titanium.
It is characterized using pattern of the transmission electron microscope to petal spherical carbide titanium obtained by Examples 1 to 4, Fig. 3 pairs
The petal spherical carbide titanium for answering embodiment 2 to obtain, from the figure 3, it may be seen that the present embodiment resulting materials are what relatively thin nanometer sheet was constituted
Floriform appearance, nanometer sheet with a thickness of 20~30nm.The pattern and embodiment 2 of embodiment 1,3 and 4 gained petal spherical carbide titaniums
It is similar.
Using BET specific surface area method of testing/specific surface and Porosimetry (AutosorbiQ, U.S. Kang Ta) to embodiment
The pore structure and specific surface area of 1~4 gained petal spherical carbide titanium are characterized, and characterization result is shown obtained by Examples 1 to 4
The pore-size distribution of petal spherical carbide titanium belongs to typical meso-hole structure in the section 20~50nm；Petal obtained by Examples 1 to 4
The specific surface area of spherical carbide titanium is approximately 29m respectively2·g-1、36m2·g-1、33m2·g-1And 38m2·g-1。
It is characterized using structure of the X-ray diffractometer to petal spherical carbide titanium obtained by Examples 1 to 4.Fig. 4 is corresponding real
Apply the XRD diagram of 3 gained petal spherical carbide titanium of example, four main feature diffraction maximums in XRD diagram respectively with Ti3C2Mxene's
(002), (004), (006) are corresponding with (110) crystal face, show that resulting materials of the present invention are Ti3C2Mxene (titanium carbide two-dimensional layer
Structure).The characterization result of embodiment 1,2 and 4 shows that resulting materials of the present invention are Ti3C2Mxene structure.
By petal spherical carbide titanium obtained by Examples 1 to 4 and dehydrated alcohol according to 5mg titanium carbide: 10mL dehydrated alcohol
Mass ratio is prepared by mixing into slurry, is modified by physical absorption (i.e. drop coating in the way of) glass-carbon electrode, using three electrodes
System carries out electrochemical impedance test, the test result of Fig. 5 corresponding embodiment 3, as seen from Figure 5 petal ball to modified electrode
Shape Ti3C2In the nyquist plot of Mxene modified glassy carbon electrode, half circular diameter is far smaller than bare glassy carbon electrode, shows the present invention
The petal spherical shape Ti of preparation3C2Mxene material has excellent metallic conductivity and electro-chemical activity.The survey of embodiment 1,2 and 4
Test result is close with embodiment 3, and petal spherical carbide titanium electrochemical impedance test resistance value provided by the invention is lower than 30 Ω, material
Material has excellent electric conductivity.
In ethanol by the dispersion of petal spherical carbide titanium obtained by Examples 1 to 4, wherein embodiment 1 is by 20mg to the present invention
Petal spherical carbide titanium is dispersed in the ethyl alcohol of 30mL, and embodiment 2 is that 20mg petal spherical carbide titanium is dispersed in 50mL ethyl alcohol,
Embodiment 3 and 4 is dispersed in the ethyl alcohol of 40mL with the petal spherical carbide titanium of 20mg, to characterize the dispersion of petal spherical carbide titanium
Property.The test result of 4 gained petal spherical carbide titanium of Fig. 6 corresponding embodiment, it will be appreciated from fig. 6 that the alcohol of petal spherical carbide titanium point
Dispersion liquid disperses uniform, no obvious sediment, and dispersion liquid is in light gray；It places after two weeks, still without significant change, it was demonstrated that the present invention
The petal spherical carbide titanium of offer can be with mass production.Examples 1 to 3 test result and embodiment 4 are same, and it is equal to obtain dispersion
One, the light grey dispersion liquid of no obvious sediment.
As seen from the above embodiment, the nanometer sheet in petal spherical carbide titanium provided by the invention is thinner, only 20~
30nm, increases the large specific surface area of material, and meso-hole structure is also beneficial to promote the electro-chemical activity of material, therefore, can be
Hydrogen storage, lithium ion battery, electro-catalysis, supercapacitor and sensor field application.
The present invention uses different organic solvents intercalation Ti3C2, and using ultrasonic wave added method prepare it is petal-like
Ti3C2Mxene material, increases Ti3C2Interfloor distance, the process of removing is more efficient, and operating procedure is simple, low in cost；Nothing
Complicated equipment is needed, can be mass produced, realizes industrialization.
Although above-described embodiment is made that detailed description to the present invention, it is only a part of the embodiment of the present invention,
Rather than whole embodiments, people can also obtain other embodiments under the premise of without creativeness according to the present embodiment, these
Embodiment belongs to the scope of the present invention.
Claims (10)
1. a kind of petal spherical carbide titanium, by being constituted with a thickness of the nanometer sheet of 20~30nm；The petal spherical carbide titanium has
Hole, the aperture of hole are 20~50nm；The partial size of the petal spherical carbide titanium is 200~300nm.
2. petal spherical carbide titanium as described in claim 1, which is characterized in that the specific surface area of the petal spherical carbide titanium
For 28~40m2·g-1。
3. the preparation method of petal spherical carbide titanium as claimed in claim 1 or 2, comprising the following steps:
(1) under agitation, by Ti3AlC2Powder is added in hydrofluoric acid solution, and titanium carbide is obtained after etching；
(2) it under ultrasound condition, is removed, is spent using the titanium carbide that different intercalators obtains the step (1)
Valve spherical carbide titanium；
The intercalator includes N,N-dimethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide or acetonitrile.
4. preparation method as claimed in claim 3, which is characterized in that Ti in the step (1)3AlC2Partial size≤300 of powder
Mesh.
5. preparation method as claimed in claim 3, which is characterized in that the mass concentration of hydrofluoric acid solution in the step (1)
It is 10~30%.
6. preparation method as claimed in claim 3 or 5, which is characterized in that Ti in the step (1)3AlC2The quality and hydrogen of powder
Volume ratio >=1g:10mL of fluorspar acid solution.
7. the preparation method as described in claim 3,4 or 5, which is characterized in that Ti in the step (1)3AlC2The addition speed of powder
Degree is 0.1~0.5g/min.
8. the preparation method as described in claim 3,4 or 5, which is characterized in that the time etched in the step (1) is 24~
48h。
9. preparation method as described in claim 1, which is characterized in that in the step (2) ultrasonic power be 180~
240W；Ultrasound time be 8~for 24 hours.
10. the preparation method preparation of any one of petal spherical carbide titanium of any of claims 1 or 2 or claim 3~9
Application of the obtained petal spherical carbide titanium in hydrogen storage, lithium ion battery, electro-catalysis, supercapacitor or sensor field.
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