CN103641119B - The preparation method of one kind grapheme material - Google Patents
The preparation method of one kind grapheme material Download PDFInfo
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- CN103641119B CN103641119B CN201310635182.5A CN201310635182A CN103641119B CN 103641119 B CN103641119 B CN 103641119B CN 201310635182 A CN201310635182 A CN 201310635182A CN 103641119 B CN103641119 B CN 103641119B
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- ultrasonic disperse
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- grapheme material
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Abstract
The invention discloses a kind of to Ti
3alC
2carry out selective etch to prepare the method for class grapheme material: by Ti
3alC
2cross 100 ~ 200 mesh sieves, by Ti under magnetic agitation or ultrasonic disperse
3alC
2put into hydrofluoric acid solution and react 20h, reaction product ethanol and distilled water repetitive scrubbing is clean, then ultrasonic disperse 1 ~ 6h, then carry out centrifugal or suction filtration, by the product dry 1 ~ 2h at 50 DEG C collected.Method cost of the present invention is low, and technique is simple, easy to operate, is applicable to being extended to industrial production.
Description
Technical field
The present invention relates to nano-functional material field, particularly, to Ti
3alC
2carry out selective etch to prepare the method for class grapheme material.
Background technology
Graphene is a kind of New Two Dimensional plane nano material be just found for 2004, its special monoatomic layer structures shape it there is the abundant and physical properties of novelty. become from once finding into Graphene the international forward position and focus that get most of the attention.
Although Graphene has won more concern than other two-dimensional material, simple chemical bond and weak Van der Waals key have limited its application between layers; In general, the stratified material of multielement has how potential character than the material of single element, because the material of multielement has more compositional variable, can realize more how special character.
MAX phase is hexagonal system (the spacer P6 of layered arrangement
3/ mmc), each structure cell has two molecules.Staggered being connected with pure A atomic shell of compact arranged M layer, X atom fills the octahedral interstices of M.M
n+1aX
nthe ternary layered carbide of general formula and nitride are all have anisotropic laminate structure (n=1,2, or 3, M is early transition metal, and A is Al and Si mainly, and X is C and N mainly).The nearly kind more than 60 of MAX phase of current discovery; Ti
3alC
2the class that in MAX phase, research is the most very promising, Ti
3alC
2be a kind of novel lamellar ternary compound, it is with metal and ceramic many advantages, as conduction, the thermal conductivity of excellence, and workability, good survivability, the advantages such as high-melting-point, high-modulus, high strength and low density; M
n+1x
nstratification Nature comparison is stablized, and the connecting key of A layer is relatively weak, and reactive behavior is also stronger; The mechanical deformation of MAX phase is subject to the impact of substrate dislocation, and has anisotropy, and the demixing phenomenon of deformation meeting generating portion, can form the thin slice of about tens or hundreds of nanometer, namely easy from Ti
3alC
2in detach Al layer and form a kind of New Two Dimensional material, and the potential using value of similar Graphene can be had also to maintain the performance of some excellences of MAX phase; Domestic at present do not have Ti
3alC
2carry out the relevant report that selective corrosion becomes class graphene-structured, external Naguib team is undertaken being obtained by reacting two-dirnentional structure by hydrothermal method, but leaving standstill makes particle easily reunite, and the particle erosion effect be deposited on below is not thorough, the present invention carries out at normal temperatures, is more suitable for being generalized to industrial production, and the concentration of acid used is lower, in order to solve the uneven shortcoming of corrosion, stirring or ultrasonic method in reaction process, is adopted to make reaction uniform and complete more.
Summary of the invention
The object of the present invention is to provide a kind of to Ti
3alC
2carry out selective etch to prepare the method for class grapheme material, develop a kind of novel Graphene and replace material.
Above-mentioned purpose is achieved by the following technical solution: by Ti
3alC
2in HF acid, carry out chemical etching, Al is etched away by selectivity, form a kind of two-dimensional material, particularly, comprise the steps:
(1) by Ti
3alC
2clay into power, sieve under 100 ~ 200 object sub-sieves, obtain evenly tiny particle in case cause because particle is excessive corrosion not thorough;
(2) under magnetic agitation or ultrasonic disperse by Ti
3alC
2put into hydrofluoric acid solution and react 20h; The concentration of hydrofluoric acid solution is commercially available the most frequently used concentration 40wt%, according to stoichiometric and make whole reaction process hydrofluoric acid hold certain corrosion strength, adds 1 ~ 3g Ti in every 40 ~ 60ml hydrofluoric acid solution
3alC
2;
(3) after product ethanol and distilled water repetitive scrubbing will be reacted clean, then ultrasonic disperse 1 ~ 6h, be separated with the synusia connected with weak van der waals forces again after ensureing to corrode;
(4) then scattered product is carried out centrifugal or collected by suction, by product dry 1 ~ 2 h at 50 DEG C collected.
Effect of the present invention and advantage:
Ti
3alC
2preparation technology simple, cost is low, only can successfully prepare high-purity product with conventional raw material; The chemical etching that HF is right just can carry out at normal temperatures, and mild condition is easy to operate; Generate product and both maintain Ti
3alC
2performance, show again the character being similar to Graphene, very potential Graphene equivalent material can be become.
Accompanying drawing explanation
Fig. 1 is Ti
3alC
2the enlarged view of the SEM of the product of chemical etching different time and TEM image: a is 6 h, b in HF acid be 12 h, c to be 20 h, d be c, e is the TEM figure of the product of chemical etching 20 h.
Fig. 2 is Ti
3alC
2xRD correlation curve before and after chemical etching 20 h.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
embodiment 1:
By Ti
3alC
2clay into power, sieve under 200 object sub-sieves, obtain being less than the even grain of 200 object, by 2.5g Ti under magnetic agitation or ultrasonic disperse
3alC
2put into 60ml 40% hydrofluoric acid solution and react 6h, it is clean to react after product ethanol and distilled water repetitive scrubbing, then ultrasonic disperse 3h, then scattered product is carried out centrifugal or collected by suction, by the product dry 2h at 50 DEG C collected.
embodiment 2:
By Ti
3alC
2clay into power, sieve under 200 object sub-sieves, obtain being less than the even grain of 200 object, by 2.5g Ti under magnetic agitation or ultrasonic disperse
3alC
2put into 60ml 40% hydrofluoric acid solution and react 12h, it is clean to react after product ethanol and distilled water repetitive scrubbing, then ultrasonic disperse 3h, then scattered product is carried out centrifugal or collected by suction, by the product dry 1h at 50 DEG C collected.
embodiment 2:
By Ti
3alC
2clay into power, sieve under 200 object sub-sieves, obtain being less than the even grain of 200 object, by 2.5g Ti under magnetic agitation or ultrasonic disperse
3alC
2put into 60ml 40% hydrofluoric acid solution and react 20h, it is clean to react after product ethanol and distilled water repetitive scrubbing, then ultrasonic disperse 3h, then scattered product is carried out centrifugal or collected by suction, by the product dry 2h at 50 DEG C collected.
embodiment 3
By Ti
3alC
2clay into power, sieve under 200 object sub-sieves, obtain being less than the even grain of 200 object, by 2.5g Ti under magnetic agitation or ultrasonic disperse
3alC
2put into 60ml 40% hydrofluoric acid solution and react 20h, it is clean to react after product ethanol and distilled water repetitive scrubbing, then ultrasonic disperse 1h, then scattered product is carried out centrifugal or collected by suction, by the product dry 2h at 50 DEG C collected.
embodiment 4
By Ti
3alC
2clay into power, sieve under 200 object sub-sieves, obtain being less than the even grain of 200 object, by 2.5g Ti under magnetic agitation or ultrasonic disperse
3alC
2put into 60ml 40% hydrofluoric acid solution and react 20h, after product ethanol and the clean ultrasonic disperse 2h again of distilled water repetitive scrubbing will be reacted, then scattered product is carried out centrifugal or collected by suction, by the product dry 2h at 50 DEG C collected.Product after washing is carried out ultrasonic disperse, and the different dispersion effect of jitter time is different, and the effect of ultrasonic 2h is best.
As accompanying drawing 1; Find along with the reaction times increases by changing right chemical etching time, constantly and interlaminar separation, layer and layer divide Al gradually, are separated, and formation thin slice, when etching time substantially no longer changes more than 20h after product pattern, therefore etching time elects 20h as.Accompanying drawing 2 is Ti
3alC
2xRD correlation curve before and after chemical etching 20h.Can find out that from figure the structure before and after etching has a very large change, the direction of chemical etching is along the direction of (002), and the interlaminar separation caused, makes structure expand along c-axis, reaches platelet exfoliation by ultrasonic further.
Claims (4)
1. the preparation method of a kind grapheme material, is characterized in that comprising the steps:
(1) by Ti
3alC
2clay into power, sieve, obtain evenly tiny particle in case cause because particle is excessive corrosion not thorough;
(2) under magnetic agitation or ultrasonic disperse by Ti
3alC
2put into hydrofluoric acid solution and react 20h; 1 ~ 3g Ti is added in every 40 ~ 60ml hydrofluoric acid solution
3alC
2;
(3) will to react after after product washes clean ultrasonic disperse again, be separated with the synusia connected with weak van der waals forces again after ensureing to corrode, the time of described ultrasonic disperse is 2h;
(4) then scattered product is carried out centrifugal or collected by suction, by dry for the product collected.
2. the preparation method of a kind grapheme material as claimed in claim 1, is characterized in that: described in sieve and referred to 100 ~ 200 object sub-sieves.
3. the preparation method of a kind grapheme material as claimed in claim 1, is characterized in that: the concentration 40wt% of described hydrofluoric acid solution.
4. the preparation method of a kind grapheme material as claimed in claim 1, is characterized in that: described drying refers to dry 1 ~ 2 h at 50 DEG C.
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|---|---|---|---|
| CN201310635182.5A CN103641119B (en) | 2013-12-03 | 2013-12-03 | The preparation method of one kind grapheme material |
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| CN103641119A CN103641119A (en) | 2014-03-19 |
| CN103641119B true CN103641119B (en) | 2015-10-28 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016345B (en) * | 2014-06-03 | 2016-04-27 | 河海大学 | The preparation method of one kind Graphene two-dimensional layer titanium carbide nanometer sheet |
| CN104072868B (en) * | 2014-06-12 | 2017-02-15 | 宁波信远石墨有限公司 | Graphene-like modified thermal conductive plastic and preparation method thereof |
| CN104587947A (en) * | 2014-12-23 | 2015-05-06 | 陕西科技大学 | Method for preparing two-dimensional nano-adsorbent titanium carbide for effectively adsorbing hexavalent chromium ions |
| CN104495918B (en) * | 2014-12-23 | 2016-05-25 | 陕西科技大学 | The preparation method of particulate titanium dioxide/two-dimensional nano titanium carbide composite |
| CN104549149A (en) * | 2014-12-23 | 2015-04-29 | 陕西科技大学 | Preparation method of two-dimensional adsorbent titanium carbide for effectively treating potassium permanganate solution |
| CN104528721A (en) * | 2014-12-23 | 2015-04-22 | 陕西科技大学 | Preparation method of flaky two-dimensional nano-titanium carbide nanometre material |
| CN104496461B (en) * | 2014-12-23 | 2016-05-25 | 陕西科技大学 | The preparation method of cubic titanium dioxide/two-dimensional nano titanium carbide composite |
| CN104576850B (en) * | 2015-01-16 | 2017-02-22 | 太原理工大学 | Preparing method for light-emitting diode of vertical structure |
| CN104795252B (en) * | 2015-03-27 | 2017-06-20 | 中国科学院金属研究所 | Ultra-thin Ti3C2The preparation method of the electrode of super capacitor of nanometer sheet self assembly |
| CN104882603B (en) * | 2015-04-24 | 2017-06-09 | 中南大学 | Nano-micro structure lithium ion battery negative material Ti2C microballoons and preparation method thereof |
| CN104821401B (en) * | 2015-05-12 | 2017-05-17 | 中南大学 | Two-dimensional lithium ion battery additive VC2 nanosheet and preparation method thereof |
| CN104817083A (en) * | 2015-05-25 | 2015-08-05 | 哈尔滨工业大学 | Rapid-heating-assisted ultrasonic stripping method for two-dimensional nanometer Ti3C2 lamella |
| CN109052548A (en) * | 2018-07-23 | 2018-12-21 | 大连理工大学 | A kind of method of ultraviolet catalytic processing waste water from dyestuff |
| CN111715182A (en) * | 2020-05-18 | 2020-09-29 | 中国石油天然气股份有限公司 | Oil-removing carbon fiber pipe sponge and preparation and application methods thereof |
-
2013
- 2013-12-03 CN CN201310635182.5A patent/CN103641119B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| Synthesis of a new graphene-like transition metal carbide by de-intercalating Ti3AlC2;Fangyuan Chang et al.;《Materials Letters》;20130802;第109卷;第295页-第298页 * |
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