CN107416781A - A kind of two-dimentional titanium nitride carbon nano-tube compound film and preparation method thereof - Google Patents
A kind of two-dimentional titanium nitride carbon nano-tube compound film and preparation method thereof Download PDFInfo
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- CN107416781A CN107416781A CN201710614506.5A CN201710614506A CN107416781A CN 107416781 A CN107416781 A CN 107416781A CN 201710614506 A CN201710614506 A CN 201710614506A CN 107416781 A CN107416781 A CN 107416781A
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a kind of two-dimentional titanium nitride carbon nano-tube compound film and preparation method thereof, belong to field of membrane preparation.This method comprises the following steps：（1）First acid solution and lithium salts are mixed, add Ti4AlN3Powder, stir, centrifuge, dry, you can obtain Ti4N3Powder；（2）By Ti4N3Powder mixes with water, ultrasound, you can obtain Ti4N3Nanometer sheet solution；（3）By Ti4N3Nanometer sheet solution mixes with carbon nano-tube solution, stirring, then by self-assembling technique, is stacked on perforated substrate, a kind of two-dimentional titanium nitride carbon nano-tube compound film is can obtain after drying.Two-dimentional titanium nitride carbon nano-tube compound film tool good conductivity prepared by the present invention, mechanical performance are excellent；The preparation method of the composite membrane is simple, easy to operate, energy consumption is low, cost is low, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to membrane material preparation field, and in particular to a kind of two-dimentional titanium nitride-carbon nano-tube compound film and its system
Preparation Method.
Background technology
Since graphene comes out, various two-dimensional materials are gradually explored and have developed by people.Such as
Boron nitride, Transition-metal dichalcogenide, layered metal oxide, black squama alkene, transition metal carbon（Nitrogen）Compound etc..Two-dimentional material
Material generally has preferable heat endurance, excellent mechanical performance and the compatibility with polymer or other materials.Therefore,
Other materials and two-dimensional material is compound in recent years and one of study hotspot.A kind of New Two Dimensional material MXene, also by people
It has developed in 2011, compared with graphene, MXene material synthesis processes are simpler, water-soluble more preferable, and electric conductivity is also more
It is excellent, and the composite of graphene and other materials has widely been developed, and it is applied to every field.Such as
Graphene/carbon nano-tube composite membrane has been widely used in lithium ion battery, sodium-ion battery, lithium-sulfur cell, lithium air electricity
The fields such as pond, ultracapacitor and electro-catalysis.However, in view of MXene excellent properties, MXene and CNT it is compound
With good application prospect, MXene families are huge, however, there is presently no people by Ti4N3This MXene enters with CNT
Row is compound to prepare composite membrane.
Therefore, how to prepare two-dimentional titanium nitride/carbon nano-tube compound film in a simple way becomes study hotspot.
The content of the invention
In order to improve existing technology, it is an object of the invention to provide a kind of two-dimentional titanium nitride-carbon nano-tube compound film and
Its preparation method.
The object of the invention is achieved through the following technical solutions.
A kind of preparation method of two-dimentional titanium nitride-carbon nano-tube compound film, comprises the following steps：
（1）Acid solution is mixed with lithium salts, obtains mixed liquor；Then by Ti4AlN3Powder is added in mixed liquor, is stirred,
Centrifuge washing, dry, obtain Ti4N3Powder；
（2）By Ti4N3Powder is dissolved in the water, and ultrasound is uniformly, you can obtains two-dimentional Ti4N3Nanometer sheet solution；
（3）By two-dimentional Ti4N3Nanometer sheet solution mixes with carbon nano-tube solution, stirring, then by self-assembling technique, is stacked into more
In the substrate of hole, two-dimentional titanium nitride-carbon nano-tube compound film is obtained after drying.
Preferably, step（3）Described two-dimentional Ti4N3The concentration of nanometer sheet solution is 0.01 ~ 1 mg/ml.
Preferably, step（3）Described two-dimentional Ti4N3The dosage of nanometer sheet solution is 1 ~ 100ml.
Preferably, step（3）The concentration of described carbon nano-tube solution is 0.1 ~ 5 mg/ml.
Preferably, step（3）The dosage of described carbon nano-tube solution is 1 ~ 50ml.
Preferably, step（3）Described self-assembling technique is in spin coating method, natural seasoning and vacuum filtration method
More than one.
Preferably, step（3）Described substrate is anodised aluminium filter membrane（AAO）With one kind in mixed cellulose ester membrane
More than.
Preferably, step（3）The drying is one or more of air dry oven drying and vacuum drying；The drying
Temperature be 30 DEG C ~ 100 DEG C, the dry time be 2 ~ 36 hours.
Preferably, step（1）In, described acid solution is one or more of hydrochloric acid, sulfuric acid and nitric acid；Described lithium salts
For more than one in lithium fluoride, lithium chloride and lithium bromide；The volume mass ratio of the acid solution and lithium salts is 200mL：（1~
10g）.
Preferably, step（1）In, the temperature of described stirring is 50 ~ 200 DEG C.
Preferably, step（1）In, the volumetric concentration of the acid solution is 2% ~ 50%.
Preferably, step（1）Described in Ti4AlN3The quality of powder is 2g ~ 50g.
Preferably, step（1）Described in the time to stir be 10 ~ 72 hours.
Preferably, step（1）Described in the rotating speed that stirs be 20 ~ 1000rpm；The rotating speed of centrifugation is 200 ~ 5000 rpm；
The time of centrifugation is 50 ~ 200 min.
Preferably, step（1）Described in drying condition for air dry oven is dry, one kind or one kind in vacuum drying
More than；Described drying temperature is 50 DEG C ~ 100 DEG C；The dry time is 10 ~ 72 hours.
It is further preferred that step（2）Described in Ti4N3The mass volume ratio of powder and water is 1g：（1~100）ml.
Preferably, step（2）Described in ultrasonic time be 1 ~ 5 hour.
A kind of two-dimentional titanium nitride-carbon nano-tube compound film, the electric conductivity of the composite membrane as made from the process described above
Good, electrical conductivity is up to 4500 ~ 4600 S/cm, and mechanical performance is excellent.
The present invention is by by two-dimensional material Ti4N3It is compound with carbon nano-tube solution progress, prepare Ti4N3- CNT
Composite membrane is expected to be applied to lithium ion battery, sodium-ion battery, lithium-sulfur cell, lithium-air battery, ultracapacitor, electro-catalysis etc.
Field.
Compared with prior art, the invention has the advantages that：
（1）Ti in two-dimentional titanium nitride-carbon nano-tube compound film of the present invention4N3Compound uniformly with CNT, CNT is very
Good is inserted into Ti4N3Among the interlayer of nanometer sheet.
（2）Preparation method of the invention is simple, easy to operate, energy consumption is low, cost is low, can greatly save in actual applications
Cost, it is adapted to large-scale industrial production.
（3）The good conductivity of two-dimentional titanium nitride-carbon nano-tube compound film of the present invention, mechanical performance is excellent, can carry out
Folding, the bending of wide-angle, are expected to be applied to lithium ion battery, sodium-ion battery, lithium-sulfur cell, lithium-air battery, super electricity
The field such as container and electro-catalysis, favorable repeatability, it is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the surface Scanning Electron microscope figure of two-dimentional titanium nitride-carbon nano-tube compound film prepared by embodiment 1；
Fig. 2 is the cross sectional Scanning Electron microscope figure of two-dimentional titanium nitride-carbon nano-tube compound film made from embodiment 2.
Embodiment
It is described further with reference to example and specific implementation of the accompanying drawing to the present invention, but embodiments of the present invention are not
It is limited to this.
Embodiment 1
A kind of preparation method of two-dimentional titanium nitride-carbon nano-tube compound film, comprises the following steps：
（1）First by 200ml hydrochloric acid solutions（Volumetric concentration 10%）Mixed with 1g lithium fluoride, then by 2g Ti4AlN3Powder is added to
In above-mentioned solution, 10h is stirred at 50 DEG C, the centrifuge washing under 20rpm, dries, obtains Ti4N3Powder；
（2）By 1g Ti4N3Powder mixes with 1 ml deionized waters, ultrasonic 1h, obtains two-dimentional Ti4N3Nanometer sheet solution, concentration are
1mg/ml；
（3）Take 0.5ml above-mentioned two-dimentional Ti4N3Nanometer sheet solution, the carbon nano-tube solution that 1ml concentration is 0.1 mg/ml is added,
10min is stirred, by vacuum filtration, is stacked on AAO perforated substrates, two-dimentional titanium nitride-carbon is can obtain after 30 DEG C of dry 2h
Nanometer tube composite film.
The surface Scanning Electron microscope of two-dimentional titanium nitride-carbon nano-tube compound film manufactured in the present embodiment（SEM）Figure is shown in
Fig. 1.It can be found that CNT and Ti in the composite membrane from figure4N3Nanometer sheet is well mixed, meanwhile, its electrical conductivity is up to
4500 S/cm。
Embodiment 2
A kind of preparation method of two-dimentional titanium nitride-carbon nano-tube compound film, comprises the following steps：
（1）First by 200ml salpeter solutions（Volumetric concentration 50%）Mixed with 10g lithium bromides, then by 20g Ti4AlN3Powder adds
Into above-mentioned solution, 20h is stirred at 100 DEG C, at 500 rpm centrifuge washing, dry, obtain Ti4N3Powder；
（2）By 1g Ti4N3Powder mixes with 100ml deionized waters, ultrasonic 5h, obtains two-dimentional Ti4N3Nanometer sheet solution, concentration are
0.01mg/ml；
（3）Take 50ml above-mentioned two-dimentional Ti4N3Nanometer sheet solution, the carbon nano-tube solution that 25ml concentration is 5 mg/ml is added, is stirred
10min is mixed, by spontaneously drying, is stacked on mixed cellulose ester perforated substrate, two dimension is can obtain after 100 DEG C of dry 24h
Titanium nitride-carbon nano-tube compound film.
The surface Scanning Electron microscope of two-dimentional titanium nitride-carbon nano-tube compound film manufactured in the present embodiment（SEM）Figure is shown in
Fig. 2.CNT is uniformly inserted into Ti in the composite membrane4N3Among the interlayer of nanometer sheet, meanwhile, its electrical conductivity is up to
4500 S/cm。
Embodiment 3
A kind of preparation method of two-dimentional titanium nitride-carbon nano-tube compound film, comprises the following steps：
（1）First by 200ml sulfuric acid solutions（Volumetric concentration 40%）Mixed with 5g lithium bromides, then by 10g Ti4AlN3Powder is added to
In above-mentioned solution, 10h is stirred at 80 DEG C, at 800 rpm centrifuge washing, dry, obtain Ti4N3Powder；
（2）By 1g Ti4N3Powder mixes with 10ml deionized waters, ultrasonic 3h, obtains two-dimentional Ti4N3Nanometer sheet solution, concentration are
0. 1mg/ml；
（3）Take 20ml above-mentioned two-dimentional Ti4N3Nanometer sheet solution, the carbon nano-tube solution that 15ml concentration is 2.5 mg/ml is added,
10min is stirred, by vacuum drying, is stacked on mixed cellulose ester perforated substrate, two dimension is can obtain after 80 DEG C of dry 14h
Titanium nitride-carbon nano-tube compound film.
Two-dimentional titanium nitride-carbon nano-tube compound film electrical conductivity manufactured in the present embodiment is up to 4500 S/cm, and mechanical performance is good
It is good, folding, the bending of wide-angle can be carried out.
Claims (10)
1. a kind of preparation method of two-dimentional titanium nitride-carbon nano-tube compound film, it is characterised in that comprise the following steps：
（1）Acid solution is mixed with lithium salts, obtains mixed liquor；Then by Ti4AlN3Powder is added in mixed liquor, is stirred, from
The heart washs, and dries, obtains Ti4N3Powder；
（2）By Ti4N3Powder is dissolved in the water, and ultrasound is uniformly, you can obtains two-dimentional Ti4N3Nanometer sheet solution；
（3）By two-dimentional Ti4N3Nanometer sheet solution mixes with carbon nano-tube solution, stirring, then by self-assembling technique, is stacked into more
In the substrate of hole, two-dimentional titanium nitride-carbon nano-tube compound film is obtained after drying.
2. preparation method according to claim 1, it is characterised in that step（1）The temperature of the stirring is 50 ~ 200 DEG C,
Time is 10 ~ 72 hours.
3. preparation method according to claim 1, it is characterised in that step（1）In, described acid solution is hydrochloric acid, sulphur
One or more of acid and nitric acid；Described lithium salts is more than one in lithium fluoride, lithium chloride and lithium bromide；The acid solution with
The volume mass ratio of lithium salts is 200mL：（1~10g）.
4. preparation method according to claim 1, it is characterised in that step（3）Described two-dimentional Ti4N3Nanometer sheet solution
Concentration be 0.01 ~ 1 mg/ml.
5. preparation method according to claim 1, it is characterised in that step（3）Described two-dimentional Ti4N3Nanometer sheet solution
Dosage be 1 ~ 100ml.
6. preparation method according to claim 1, it is characterised in that step（3）The concentration of described carbon nano-tube solution
For 0.1 ~ 5 mg/ml.
7. preparation method according to claim 1, it is characterised in that step（3）The dosage of described carbon nano-tube solution
For 1 ~ 50ml.
8. preparation method according to claim 1, it is characterised in that step（3）Described self-assembling technique applies for rotation
Cover one or more of method, natural seasoning and vacuum filtration method.
9. preparation method according to claim 1, it is characterised in that step（3）The drying is dried for air dry oven
With vacuum drying one or more of；The temperature of the drying is 30 DEG C ~ 100 DEG C, and the dry time is 2 ~ 36 hours.
A kind of 10. two-dimentional titanium nitride-carbon nano-tube compound film as made from the method described in claim any one of 1-9.
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Cited By (4)
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| CN109569317A (en) * | 2018-12-12 | 2019-04-05 | 浙江工业大学 | A kind of preparation method of MXene nanofiltration membrane |
| CN109671576A (en) * | 2018-12-12 | 2019-04-23 | 福建翔丰华新能源材料有限公司 | Carbon nano tube-MXene composite three-dimensional porous carbon material and preparation method thereof |
| CN112808024A (en) * | 2021-01-06 | 2021-05-18 | 北京工业大学 | MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration and preparation method thereof |
| CN113555547A (en) * | 2021-08-10 | 2021-10-26 | 大连理工大学 | Preparation and application of positive carbon-based membrane material for lithium-sulfur battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569317A (en) * | 2018-12-12 | 2019-04-05 | 浙江工业大学 | A kind of preparation method of MXene nanofiltration membrane |
| CN109671576A (en) * | 2018-12-12 | 2019-04-23 | 福建翔丰华新能源材料有限公司 | Carbon nano tube-MXene composite three-dimensional porous carbon material and preparation method thereof |
| CN109569317B (en) * | 2018-12-12 | 2022-03-18 | 浙江工业大学 | Preparation method of MXene nanofiltration membrane |
| CN112808024A (en) * | 2021-01-06 | 2021-05-18 | 北京工业大学 | MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration and preparation method thereof |
| CN112808024B (en) * | 2021-01-06 | 2022-11-04 | 北京工业大学 | MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration and preparation method thereof |
| CN113555547A (en) * | 2021-08-10 | 2021-10-26 | 大连理工大学 | Preparation and application of positive carbon-based membrane material for lithium-sulfur battery |
| CN113555547B (en) * | 2021-08-10 | 2022-12-09 | 大连理工大学 | Preparation and application of positive carbon-based membrane material for lithium-sulfur battery |
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Application publication date: 20171201 |