CN106185936A - A kind of utilize ammonia intercalation, peel off two dimensional crystal titanium carbide nano material method - Google Patents
A kind of utilize ammonia intercalation, peel off two dimensional crystal titanium carbide nano material method Download PDFInfo
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- CN106185936A CN106185936A CN201610536766.0A CN201610536766A CN106185936A CN 106185936 A CN106185936 A CN 106185936A CN 201610536766 A CN201610536766 A CN 201610536766A CN 106185936 A CN106185936 A CN 106185936A
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- titanium carbide
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- 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
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- 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
- C01P2002/78—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by stacking-plane distances or stacking sequences
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The present invention relates to a kind of utilize ammonia intercalation, peel off two dimensional crystal titanium carbide nano material method, two dimensional crystal titanium carbide material is joined in ammonia, utilize high-speed shearing machine to carry out intercalation, stripping, then obtain, after cleaned, vacuum drying, the two dimensional crystal titanium carbide nano material that interlamellar spacing increases.The two dimensional crystal titanium carbide nano material interlamellar spacing of the present invention is relatively big, can to a certain degree overcome the reuniting effect between titanium carbide, increase its specific surface area, improve its performance at aspects such as ultracapacitor, lithium ion battery, absorption.
Description
Technical field
The invention belongs to two dimensional crystal MXene field of nano material preparation, utilize ammonia intercalation, stripping particularly to one
Prepare the preparation method of large interlamellar spacing two dimensional crystal titanium carbide nano material.
Background technology
MXene material is a kind of novel two-dimentional transition metal carbide or carbonitride, has class graphene-structured, mesh
Front main by the acquisition of HF acid etch ternary layered compound MAX phase ceramics, its chemical formula is Mn+1XnTx, wherein M represents transition
Metallic element, X represents carbon or nitrogen, and Tx is-OH/=O ,-F, n=1,2,3.MXene has good electric conductivity, hydrophilic, thoroughly
Photosensitiveness, magnetic, can be applicable to the fields such as ultracapacitor, lithium ion battery, hydrogen storage, sensor.
But due to MXene layer by layer between inevitable reuniting effect, its interlamellar spacing is less, it is difficult to obtain monolayer or few layer
MXene material.Utilize organic molecule, such as hydrazine hydrate, dimethyl sulfoxide, dimethyl imide etc., as intercalating agent and point
Powder, utilizes the method for magnetic agitation to carry out intercalation processing, can increase the interlamellar spacing of MXene material significantly, to a certain degree
On overcome its reuniting effect (for example, see Nature Communications, 2013,4:1716).But the method uses
Organic substance is relatively big to people's harm, and intercalation is inefficient, and the intercalation time generally requires more than 18h.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide and a kind of simple utilize ammonia intercalation, peel off two dimension
The method of crystal titanium carbide nano material.
To this end, the invention provides a kind of utilize ammonia intercalation, peel off two dimensional crystal titanium carbide nano material method, will
Two dimensional crystal titanium carbide material joins in ammonia, utilizes high-speed shearing machine to carry out intercalation, stripping, more cleaned, vacuum drying
After obtain interlamellar spacing increase two dimensional crystal titanium carbide nano material.
Ammonia (NH3·H2O) it is common chemical reagent, cheap, less to harm.Ammonia easily decomposites NH3
And NH4 +, under external force, NH3And NH4 +Can enter in MXene lamellar spacing, increase its interlamellar spacing, play intercalation MXene
Effect.During high-speed shearing machine work, bigger shearing force can be produced.The present invention utilizes high-speed shearing machine to replace magnetic agitation
Auxiliary ammonia enters in MXene lamellar spacing, more efficiently MXene material can be carried out intercalation processing.
It is preferred that the speed of described high-speed shearing machine is 4000～8000 revs/min, described intercalation, stripping process time
Between be 1～10 hour, preferably 1～3 hour.
It is preferred that the ammonia that mass fraction is 25%～28% of 10～30ml needed for every 1g two dimensional crystal titanium carbide material
Water.
It is preferred that described vacuum drying temperature is 60～80 DEG C.
It is preferred that the method preparing two dimensional crystal titanium carbide material includes:
Pressureless sintering is used to prepare high-purity ternary layered Ti3AlC2Ceramic block, obtains Ti after milled processed3AlC2Powder body；
By gained Ti3AlC2Powder body joins in mass fraction 40%～49% Fluohydric acid., performs etching anti-at 50～70 DEG C
Answer 8～24 hours, the most cleaned and be dried, obtain described two dimensional crystal titanium carbide nano material.
Also, it is preferred that described pressureless sintering is to sinter 1～4 hour at 1300～1450 DEG C.
It is preferred that every 1gTi3AlC2Needed for powder body, 20～50ml concentration are the Fluohydric acid. of 40%～49%.
Beneficial effect:
The two dimensional crystal titanium carbide nano material interlamellar spacing of the present invention is relatively big, can to a certain degree overcome the reunion between titanium carbide
Effect, increases its specific surface area, improves its performance at aspects such as ultracapacitor, lithium ion battery, absorption；
The large interlamellar spacing two dimensional crystal titanium carbide nano material intercalation efficiency of the present invention is high, and the used time is short, easy and simple to handle, low cost,
It is prone to industrial application.
Accompanying drawing explanation
Fig. 1 a is Ti3AlC2Ti ceramic, original3C2TxThe d-Ti that (intermediate product of embodiment 1), embodiment 1 prepares3C2Tx-
2 and the prepared d-Ti of embodiment 23C2TxThe sweep limits of-10 be the sweep limits of the XRD of 5 °≤2 θ≤65 ° be 5 °≤2 θ≤
The XRD figure spectrum of 65 °；
Fig. 1 b is Ti3AlC2Ti ceramic, original3C2TxThe d-Ti that (intermediate product of embodiment 1), embodiment 1 prepares3C2Tx-2 and
The d-Ti that embodiment 2 prepares3C2TxThe sweep limits of-10 is the XRD figure spectrum of 5 °≤2 θ≤12 °；
Fig. 2 a is Ti3AlC2The SEM shape appearance figure of pottery；
Fig. 2 b is original Ti3C2TxThe SEM shape appearance figure of (intermediate product of embodiment 1)；
Fig. 2 c is the d-Ti of embodiment 1 preparation3C2TxThe SEM shape appearance figure of-2.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that following embodiment is merely to illustrate this below by way of following embodiment
Invention, and the unrestricted present invention.
The present invention, under the effect of high-speed shearing machine, utilizes ammonia to insert original two dimensional crystal titanium carbide nano material
Layer, lift-off processing, utilize deionized water fully to wash removal ammonia afterwards, and the two dimensional crystal titanium carbide obtaining interlamellar spacing increase is received
Rice material.Intercalation prepared by the present invention, peel off after two dimensional crystal titanium carbide there is bigger interlamellar spacing, can be in certain journey
Overcome the reuniting effect between two dimensional crystal titanium carbide on degree, increase specific surface area, improve it at ultracapacitor, lithium-ion electric
The performance of the aspect such as pond, absorption.
What the explanation present invention in following exemplary ground provided utilizes ammonia intercalation, peels off two dimensional crystal titanium carbide nano material
Method.
The present invention is by titanium hydride (TiH2), titanium carbide (TiC), aluminium powder (Al) is according to certain ratio (such as, mol ratio
Can be 1:2:1～1:2:1.2.) mixing, utilize ball mill ball milling a period of time (such as 12h) so that it is mix homogeneously.The most again
Tube furnace pressureless sintering is utilized to prepare high-purity ternary layered Ti3AlC2Ceramic block, processes block ceramic grinding, obtains powder body
Ti3AlC2Material.Wherein the temperature of pressureless sintering can be 1300 DEG C～1450 DEG C.The time of sintering can be 1～4 hour.
The present invention is by Ti3AlC2Powder body joins in Fluohydric acid., performs etching reaction 8～24 hours at 50～70 DEG C, after
Cleaned and be dried, obtain described two dimensional crystal titanium carbide nano material.Specifically, (such as, the present invention utilizes finite concentration
Can be 40%～49%) Fluohydric acid. (HF) selective etch Ti3AlC2Powder body.Wherein, every 1gTi3AlC2Powder body need 20～
50ml concentration is the Fluohydric acid. of 40%-49% (mass fraction).Product utilize deionized water, dehydrated alcohol fully wash
Supreme metafiltration liquid pH ≈ 7, vacuum drying obtains original two dimensional crystal titanium carbide nano material Ti3C2Tx(wherein TxFor-OH/=
O、-F).Vacuum drying temperature can be 60 DEG C～80 DEG C.
Two dimensional crystal titanium carbide material is joined in ammonia by the present invention, utilize high-speed shearing machine carry out intercalation, peel off 1～
10 hours, preferably 1～3 hour, more cleaned, after drying obtain interlamellar spacing increase two dimensional crystal titanium carbide nano material.Its
In, needed for every 1g two dimensional crystal titanium carbide material, 10～30ml mass fractions are the ammonia of 25%～28%.High-speed shearing machine
Shear rate can be 4000 revs/min～8000 revs/min.Specifically, the Ti of 5g is taken3C2Tx join equipped with 50ml～
In the beaker of 150ml ammonia (mass fraction is 25%～28%), utilize high-speed shearing machine to Ti3C2TxCarry out at intercalation, stripping
Reason, the two dimensional crystal titanium carbide then utilizing deionized water abundant washing reaction product, vacuum drying to obtain interlamellar spacing increase is received
Rice material (is expressed as d-Ti3C2Tx)。
The present invention, by high-speed shearing machine, utilizes the efficient intercalation of ammonia, stripping two dimensional crystal titanium carbide nano material.This
Bright ammonia is utilized to carry out intercalation, lift-off processing, it is to avoid the harm that human body is caused by toxic organic compound.
Two dimensional crystal titanium carbide nano material interlamellar spacing prepared by the present invention becomes big, and number of plies amount reduces, intercalation preparation method
Simple, it is easy to large-scale industrialization promotion.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Invention is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to this
Some nonessential improvement and adjustment that bright foregoing is made belong to protection scope of the present invention.Following example is concrete
Technological parameters etc. are the most only that an example in OK range, i.e. those skilled in the art can be done properly by explanation herein
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
By TiH2, TiC, Al powder in molar ratio=1:2:1.1 weigh, ball milling 12h so that it is mix homogeneously.Utilize vacuum tube furnace,
With high-purity argon gas as protective gas, 1400 DEG C of pressureless sintering 2h prepare high-purity Ti3AlC2Block materials, after grind to form 325 mesh powder
Body.8g is ground the Ti obtained3AlC2Powder body, adds the HF that concentration is 49% of 320ml, and 60 DEG C of reaction 24h, by product
Utilize deionized water, dehydrated alcohol fully to wash to supernatant PH weakly acidic pH, 80 DEG C of vacuum drying, obtain original two dimensional crystal
Titanium carbide nano material Ti3C2Tx。
Weigh Ti prepared by 5g3C2TxAdd 100ml mass fraction 25%～28% ammonia, utilize high-speed shearing machine with
The rotating speed of 6000 turns per minute, to Ti3C2Tx carries out intercalation, lift-off processing 2h, obtains the two dimensional crystal titanium carbide that interlamellar spacing increases
Nano material d-Ti3C2Tx-2.From Fig. 1 a and 1b it can be seen that with original Ti3C2TxCompare, d-Ti3C2Tx(002) of-2 samples
Peak position to low-angle offset, show that its interlamellar spacing in c direction increases, be computed its interlamellar spacing byIncrease toThe Ti of large interlamellar spacing3C2TxSuccessfully prepared.
Embodiment 2
By TiH2, TiC, Al powder in molar ratio=1:2:1.1 weigh, ball milling 12h so that it is mix homogeneously.Utilize vacuum tube furnace,
With high-purity argon gas as protective gas, 1400 DEG C of pressureless sintering 2h prepare high-purity Ti3AlC2Block materials, after grind to form 325 mesh powder
Body.8g is ground the Ti obtained3AlC2Powder body, adds in the HF that concentration is 49% of 320ml, 60 DEG C of reaction 24h, reaction is produced
Thing utilizes deionized water, dehydrated alcohol fully to wash to supernatant PH weakly acidic pH, 80 DEG C of vacuum drying, obtains original two dimensional brilliant
Body titanium carbide nano material Ti3C2Tx。
Weigh Ti prepared by 5g3C2TxAdd 100ml mass fraction 25%～28% ammonia, utilize high-speed shearing machine with
The rotating speed of 6000 turns per minute, to Ti3C2Tx carries out intercalation, lift-off processing 10h, obtains the two dimensional crystal carbonization that interlamellar spacing increases
Titanium nano material d-Ti3C2Tx-10.From Fig. 1 a and 1b it can be seen that and Ti3C2TxCompare, d-Ti3C2Tx(002) of-10 samples
Peak position to low-angle offset, show that its interlamellar spacing in c direction increases, be computed its interlamellar spacing byIncrease toThe Ti of large interlamellar spacing3C2TxSuccessfully prepared.
Fig. 2 a is Ti3AlC2The SEM shape appearance figure of pottery, Fig. 2 b is original Ti3C2TxSEM shape appearance figure, Fig. 2 c is embodiment 1
The d-Ti of preparation3C2TxThe SEM shape appearance figure of-2.Ti is can be seen that from Fig. 2 a3AlC2There is MAX phase significantly layer structure, but
It is tightly combined between its layer, through HF acid etch, Ti3AlC2In Al layer be etched away, demonstrate two-dimensional slice structure, as figure
Shown in 2b.After ammonia intercalation processing, Ti3C2TxInterlamellar spacing increase, its two-dimensional slice structure becomes apparent from, and from Fig. 2 c
It can also be seen that Ti3C2TxThe microstructure of nano material does not change.High-speed shearing machine, in this speed conditions, utilizes
During ammonia intercalation, Ti can't be destroyed3C2TxTwo-dimensional layered structure, ammonia serves increase Ti3C2TxThe effect of interlamellar spacing.
Claims (7)
1. one kind utilizes ammonia intercalation, the method peeling off two dimensional crystal titanium carbide nano material, it is characterised in that by two dimensional crystal
Titanium carbide material joins in ammonia, utilizes high-speed shearing machine to carry out intercalation, stripping, then obtains layer after cleaned, vacuum drying
The two dimensional crystal titanium carbide nano material that spacing increases.
Method the most according to claim 1, it is characterised in that the speed of described high-speed shearing machine is 4000～8000 turns/
Minute, described intercalation, the process time of stripping are 1～10 hour, preferably 1～3 hour.
Method the most according to claim 1 and 2, it is characterised in that needed for every 1g two dimensional crystal titanium carbide material 10～
30ml mass fraction is the ammonia of 25%～28%.
4. according to the method according to any one of claim 1-3, it is characterised in that described vacuum drying temperature is 60～80
℃。
5. according to the method according to any one of claim 1-4, it is characterised in that prepare the side of two dimensional crystal titanium carbide material
Method includes:
Pressureless sintering is used to prepare high-purity ternary layered Ti3AlC2Ceramic block, obtains Ti after milled processed3AlC2Powder body；
By gained Ti3AlC2Powder body joins in Fluohydric acid., carries out at 50～70 DEG C etching reaction 8～after 24 hours again through clear
Wash and be dried, obtain described two dimensional crystal titanium carbide nano material.
Method the most according to claim 5, it is characterised in that described pressureless sintering is to sinter 1 at 1300～1450 DEG C
～4 hours.
7. according to the method described in claim 5 or 6, it is characterised in that every 1g Ti3AlC2Needed for powder body, 20～50ml concentration are
The Fluohydric acid. of 40%～49%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107492455A (en) * | 2017-08-25 | 2017-12-19 | 吉林大学 | A kind of preparation method of all solid state Ehrhardt flexible miniature ultracapacitor |
| CN109192940A (en) * | 2018-08-13 | 2019-01-11 | 中南大学 | A kind of poly modified Mxene composite material and preparation method of titanium dioxide/graphene |
| CN109437172A (en) * | 2018-10-09 | 2019-03-08 | 武汉科技大学 | A kind of sodium ion intercalation Ti3C2MXene material and preparation method thereof |
| CN109692581A (en) * | 2019-01-15 | 2019-04-30 | 山东理工大学 | Two-dimensional layer Ti3C2Film and the preparation method and application thereof |
| CN110790277A (en) * | 2019-10-21 | 2020-02-14 | 上海应用技术大学 | Preparation method and application of HHK-CC @ MXenes composite flexible electrode material |
| CN111097453A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Preparation method of zirconium oxide sulfate |
| CN111533558A (en) * | 2020-02-25 | 2020-08-14 | 南京明昌新材料科技有限公司 | Pure Ti3AlC2 powder, block or porous body and preparation method and application thereof |
| CN112175275A (en) * | 2020-09-29 | 2021-01-05 | 中北大学 | Mike alkene/ethylene-vinyl acetate copolymer flexible sensing material and preparation method thereof |
| CN115151509A (en) * | 2020-02-26 | 2022-10-04 | 株式会社村田制作所 | Paste and conductive film and method for producing the same |
| CN115159451A (en) * | 2022-08-04 | 2022-10-11 | 华北电力大学（保定） | Preparation method of aluminum hydride/magnesium borohydride @ MXene composite hydrogen storage material |
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| CN107492455A (en) * | 2017-08-25 | 2017-12-19 | 吉林大学 | A kind of preparation method of all solid state Ehrhardt flexible miniature ultracapacitor |
| CN109192940B (en) * | 2018-08-13 | 2021-07-30 | 中南大学 | Titanium dioxide/graphene multi-element modified Mxene composite material and preparation method thereof |
| CN109192940A (en) * | 2018-08-13 | 2019-01-11 | 中南大学 | A kind of poly modified Mxene composite material and preparation method of titanium dioxide/graphene |
| CN109437172A (en) * | 2018-10-09 | 2019-03-08 | 武汉科技大学 | A kind of sodium ion intercalation Ti3C2MXene material and preparation method thereof |
| CN109437172B (en) * | 2018-10-09 | 2022-03-04 | 武汉科技大学 | Sodium ion intercalation Ti3C2MXene material and preparation method thereof |
| CN111097453A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Preparation method of zirconium oxide sulfate |
| CN109692581B (en) * | 2019-01-15 | 2021-08-13 | 山东理工大学 | Two-dimensional layered Ti3C2Membrane, preparation method and application thereof |
| CN109692581A (en) * | 2019-01-15 | 2019-04-30 | 山东理工大学 | Two-dimensional layer Ti3C2Film and the preparation method and application thereof |
| CN110790277A (en) * | 2019-10-21 | 2020-02-14 | 上海应用技术大学 | Preparation method and application of HHK-CC @ MXenes composite flexible electrode material |
| CN111533558A (en) * | 2020-02-25 | 2020-08-14 | 南京明昌新材料科技有限公司 | Pure Ti3AlC2 powder, block or porous body and preparation method and application thereof |
| CN115151509A (en) * | 2020-02-26 | 2022-10-04 | 株式会社村田制作所 | Paste and conductive film and method for producing the same |
| CN112175275A (en) * | 2020-09-29 | 2021-01-05 | 中北大学 | Mike alkene/ethylene-vinyl acetate copolymer flexible sensing material and preparation method thereof |
| CN115159451A (en) * | 2022-08-04 | 2022-10-11 | 华北电力大学（保定） | Preparation method of aluminum hydride/magnesium borohydride @ MXene composite hydrogen storage material |
| CN115159451B (en) * | 2022-08-04 | 2023-04-07 | 华北电力大学（保定） | Preparation method of aluminum hydride/magnesium borohydride @ MXene composite hydrogen storage material |
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Application publication date: 20161207 |