CN107522202A - A kind of stratiform two-dimensional material MXene preparation method and applications - Google Patents
A kind of stratiform two-dimensional material MXene preparation method and applications Download PDFInfo
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Abstract
The invention provides a kind of stratiform two-dimensional material MXene preparation method, comprise the following steps：S100：Ternary material M is prepared using normal pressure-sintered techniquen+1AXn, wherein M is transition metal, and A is the 3rd or the 4th major element, and X is C or N element, n 1,2, or 3；S200：By normal pressure-sintered obtained ternary material Mn+1AXnIt is ground into powder；S300：Processing is performed etching to the powder, the time of the etching processing is 8 ~ 50 hours；S400：Powder mixed liquor after etching processing is carried out to can obtain layered two-dimensional material MXene after carrying out washing treatment and drying process.The present invention instead of the flow pressurizeed in pyroprocess, reduce the threshold and complexity for preparing presoma by separating the method pressurizeed and heated.Normal pressure-sintered used equipment is more cheap in addition, and be particularly suitable for use in industrialized production.
Description
Technical field
The present invention relates to chemical preparation field, more particularly to a kind of stratiform two-dimensional material MXene preparation method.
Background technology
In the last few years, stratiform two-dimensional material（2D materials）Because of its unique property and great application potential, section is received
Boundary is ground widely to pay close attention to.From first two-dimensional material --- since graphene is found, increasing material has been added to this
Among ranks, such as boron nitride, chalcogen compound（TMDs）, some metal oxides and hydroxide etc..MXene, i.e., two
Stratiform transition metal carbide, nitride or carbonitride are tieed up, is a member newest in these materials.The material possessed
Some special natures also make its in recent years come it is of great interest.Two-dimensional metallic（Transition metal）Carbonization, carbon nitridation
Thing --- MXene was a kind of in Yury Gogotsi and the Michel W. by Drexel University in 2011
Barsoum joint researches and a kind of New Two Dimensional stratified material being prepared.It is presently classified as class graphene category,
Possess many excellent properties of graphene, such as higher specific surface area, flexible controllable component, minimum nanometer layer it is controllable with
And more excellent electric conductivity.
Equipment used in current MXene preparation technologies is complex, is unfavorable for commercial introduction, in addition current preparation
The safety coefficient of technique is relatively low, easily causes danger during operation.
The content of the invention
For above-mentioned technical problem, the invention provides a kind of new stratiform two-dimensional material MXene preparation method.This hair
Bright to prepare presoma using normal pressure-sintered, presoma is prepared and carried out at ambient pressure, by separating the method pressurizeed and heated, substitution
The flow pressurizeed in pyroprocess, reduces the threshold and complexity for preparing presoma, the preparation method can be applicable simultaneously
Largely produced in laboratory research and factory.
Technical scheme is as follows：
A kind of stratiform two-dimensional material MXene preparation method, it comprises the following steps：
S100：Ternary material M is prepared using normal pressure-sintered techniquen+1AXn, wherein M is transition metal, and A is the 3rd or the 4th main group
Element, X are C or N element, n 1,2, or 3；
S200：By normal pressure-sintered obtained ternary material Mn+1AXnIt is ground into powder；
S300：Processing is performed etching to the powder, the time of the etching processing is 8 ~ 50 hours；
S400：Powder mixed liquor after etching processing is carried out to can obtain layered two after carrying out washing treatment and drying process
Tie up material MXene.
Wherein, the step S100 specifically comprises the following steps：
S110：Weigh appropriate elemental powders；
S120：The a variety of elemental powders weighed are well mixed and carry out briquetting and handle to obtain briquetting；
S130：Normal pressure calcination processing is carried out to the briquetting and can obtain ternary material Mn+1AXn, wherein at the normal pressure calcining
The temperature of reason is 1000-1700 DEG C, and calcination time is 0.8 ~ 5 hour.
Wherein, the normal pressure calcination processing is carried out under the protection of vacuum environment or nitrogen or inert gas.
Wherein, the etching agent that etching processing uses described in step S300 is HF.
Wherein, etching agent that etching processing uses is stated in step S300 as strong acid and the mixed solution of fluoride salt.
Wherein, the strong acid is one kind of hydrochloric acid, sulfuric acid, nitric acid, perchloric acid, selenic acid, hydrobromic acid, hydroiodic acid, chloric acid etc.
Or a variety of mixture；
And/or the fluoride is lithium fluoride, potassium fluoride, sodium fluoride, one or more mixtures of ammonium acid fluoride etc..
Wherein, the etching processing is carried out under conditions of stirring.
Wherein, the carrying out washing treatment is centrifuge washing processing, to the powder carrying out washing treatment after the etching processing until molten
The pH value of liquid is 4.5 ~ 5.6.
Wherein, the drying process includes first carrying out pre-freeze processing to the sample that washing obtains afterwards, then again by described in
Processing is dried in sample at 1000-1700 DEG C.
Wherein, the M is Ti, Nb or V, A Al.
The present invention also provides stratiform two-dimensional material MXene made from above-mentioned preparation method in energy storage, electrode and adsorbing domain
Application.
The beneficial effects of the invention are as follows：
（1）The present invention prepares presoma using normal pressure-sintered method, is characterized by phase constituent and morphology characterization proves itself and heat
Press sintering finished basically identical；Method of the present invention by separating pressurization and heating, instead of the flow pressurizeed in pyroprocess,
Reduce the threshold and complexity for preparing presoma.Normal pressure-sintered used equipment is more cheap in addition, and be particularly suitable for use in work
Industry metaplasia is produced.
（2）Performed etching instead of more dangerous HF solution by strong acid mixed fluoride thing solution, examined through XRD and SEM
Survey confirms successfully to be prepared into stratiform two-dimensional material.This method acquisition Ti2C crystallinity is more preferable compared to HF caustic solutions, drops simultaneously
Low manufacturing cost, improves safe operation coefficient.
Brief description of the drawings
Fig. 1 is the normal pressure-sintered obtained ternary material Ti of embodiment one2AlC XRD；
Fig. 2 obtains Ti to be normal pressure-sintered2The SEM figures of AlC samples；
Fig. 3 is the Ti in embodiment one2The front and rear XRD spectrum comparison diagram of C etchings；
Fig. 4 is that embodiment two prepares Ti2C SEM figures；
Fig. 5 is the Ti for performing etching gained in embodiment two using HCl＆LiF mixed solutions2C XRD spectrum analysis.
Embodiment
If not otherwise indicated, the raw material used in following examples and equipment are commercially available.
Embodiment one
The present embodiment prepares stratiform two-dimensional material Ti2C.Specific preparation process is as follows：
S100：Ternary material Ti is prepared using normal pressure-sintered technique2AlC。
Wherein step S100 includes following operating procedure again：
S110：Weigh appropriate elemental powders Ti powder, pure Al powder and graphite powder；The Ti powder used in the present embodiment for (100 mesh,
Mass fraction 99.6%), pure Al powder is（200 mesh, mass fraction 99.7%）And graphite powder is（400 mesh, mass fraction
99.85%）.Concrete operations are to weigh 11.05g Ti powder；The graphite powder of 3.57g pure Al powder and 1.38g, according to atomic ratio M：
A:X is 2:1.15:1.Here the Al taken more than stoichiometric number is mainly the evaporation for preventing Al in sintering process.Need herein
Bright is that the ratios of elemental powders can be any, and it exceedes the elemental powders of stoichiometric number and in follow-up sintering and etching and washed
It can evaporate or be dissolved in solution during washing, not interfere with ternary material Ti2AlC generation.But from improve yield angle
Degree considers, according to atomic ratio M：A:X=(n+1):(1~1.8):It is more suitable that n weighs elemental powders.
S120：The a variety of elemental powders weighed are well mixed and carry out briquetting and handle to obtain briquetting.Pressed
Elemental powders preferably are used into high speed ball mill before block processing, and by mixture ball milling 5-30h, the purpose for carrying out ball-milling treatment is
Obtain evengranular mixed-powder.Briquetting processing in the present embodiment is with 10-20MPa by mixed-powder using cuber
Pressure carries out the block of compacting of the briquetting into the cm of 3 × 3 cm ~ 10 × 10.
S130：Normal pressure calcination processing is carried out to the briquetting and can obtain ternary material Ti2AlC.Specific operation process is
Briquetting is calcined using high temperature process furnances；Setting program is warming up to 1000-1700 DEG C, high temperature hold time 1-3h, forges
Whole process is burnt to carry out under vacuum conditions.
S200：By normal pressure-sintered obtained ternary material Ti2AlC is ground into powder；The briquetting after sintering is carried out first
It is broken, and reuse high speed ball mill and be milled to powder, diameter 6mm agate ball is used in the present embodiment as abrading-ball, ball
After grinding 10 h, powder sample Ti is obtained2AlC.The particle diameter of powder in step S200 is preferably less than 100 microns.
S300：Processing is performed etching to the powder using HF, the time of the etching processing is 8 hours.
The concrete operation step of etching processing is：The hydrofluoric acid solution of configuration 20%（Take 20mL hydrofluoric acid solutions（40%）, make
Diluted with 20mL deionized waters, obtain 20% hydrofluoric acid solution）.The sample that step S200 is obtained slowly is poured onto hydrogen fluorine
In acid solution（Added in magnetic agitation）To prevent bumping.Etching processing should be carried out in fume hood, in addition etching processing
It should be carried out under conditions of stirring, stirring can be ultrasonic agitation or magnetic agitation.The reaction mechanism of etching process such as lower section
Shown in journey：
Mn+1AlXn+3HF=AlF3+ Mn+1Xn +1.5H2 (1)
Mn+1Xn+2H2O =Mn+1Xn(OH)2+H2 (2)
Mn+1Xn+2HF= Mn+1XnF2+H2 (3)
（4）Powder mixed liquor after etching processing is carried out to can obtain layered two dimension after carrying out washing treatment and drying process
Material MXene.Concrete operation step is to the disperse system after etching（Powder mixed liquor）Centrifuge washing is carried out, centrifugation rate is set
For 10500 turns/min, each 8min of centrifugation time, make to be washed with deionized, until solution ph is up to 5.To carrying out washing treatment it
The sample obtained afterwards carries out 1 hour pre-freeze, is then transferred in vacuum freezing drying oven and is dried, is taken out after 18 hours, i.e.,
It can obtain stratiform two-dimensional material Ti2C。
Referring to Fig. 1, Fig. 1 is the normal pressure-sintered obtained ternary material Ti of embodiment one2AlC XRD, it is normal pressure-sintered
Obtained sample MAX-Ti2AlC is P63/mmc space lattice crystal formations.Diffraction maximum can be seen that by the contrast with standard card
Position substantially completely matches with standard card, and obtained sample can confirm as Ti2AlC；Diffraction maximum i.e. at 13 ° of 2theta
It is corresponding（0,0,2）The peak position of crystal face, peak corresponding to the crystal face are considered as Mn+1Xn characteristic peak；At about 43 ° of 2theta
It is corresponding to diffraction maximum（1,0,4）Crystal face.Fig. 2 obtains Ti to be normal pressure-sintered2The SEM figures of AlC samples.As can be seen from Figure 2
The distribution of the typical fault structure of MAX structures, further confirm by normal pressure-sintered method, successfully synthesize Ti2AlC。
Fig. 3 is Ti2The front and rear XRD spectrum contrast of C etchings.By contrasting it can be found that spreading out at about 43 ° of 2theta
Penetrate peak to disappear substantially after corrosion treatment, the peak corresponds to（1,0,4）Crystal face, it is Al characteristic peak, again shows that the corrosion
Aluminium lamination is completely exfoliated for intensity, has successfully prepared Ti2C。
A variety of analyses can successfully be prepared using normal pressure-sintered technique with surface and prepare stratiform two dimension material more than
Expect Ti2C presoma Ti2AlC, stratiform two-dimensional material Ti can be successfully prepared with reference to follow-up HF etching technics2C.Normal pressure burns
Knot technique can be carried out at ambient pressure, and up to more than 20MPa high pressure and more than 1200 DEG C need to be provided with hot pressed sintering device
High-temperature-phase ratio, greatly reduce sintering difficulty and operation difficulty, largely produced suitable for laboratory and industrialized production.
Embodiment two
The present embodiment prepares stratiform two-dimensional material Ti2C.Specific preparation process is as follows：
S100：Ternary material Ti is prepared using normal pressure-sintered technique2AlC。
Wherein step S100 includes following operating procedure again：
S110：Weigh appropriate elemental powders Ti powder, pure Al powder and graphite powder；The Ti powder used in the present embodiment for (100 mesh,
Mass fraction 99.6%), pure Al powder is（200 mesh, mass fraction 99.7%）And graphite powder is（400 mesh, mass fraction
99.85%）.
S120：The a variety of elemental powders weighed are well mixed and carry out briquetting and handle to obtain briquetting.Pressed
Elemental powders preferably are used into high speed ball mill before block processing, and by mixture ball milling 5-30h, the purpose for carrying out ball-milling treatment is
Obtain evengranular mixed-powder.Briquetting processing in the present embodiment is with 10-20MPa by mixed-powder using cuber
Pressure carries out the block of compacting of the briquetting into the cm of 3 × 3 cm ~ 10 × 10.
S130：Normal pressure calcination processing is carried out to the briquetting and can obtain ternary material Ti2AlC.Specific operation process is
Briquetting is calcined using high temperature process furnances；Setting program is warming up to 1000-1700 DEG C, high temperature hold time 1-3h, forges
Whole process is burnt to carry out under argon gas protection.
S200：By normal pressure-sintered obtained ternary material Ti2AlC is ground into powder.
S300：Processing is performed etching to the powder using HCl mixing LiF, the time of the etching processing is 36 hours.
The concrete operation step of etching processing is：30mL 6M hydrochloric acid solutions are taken, by 1.98g LiF（5mol）It is added to
Wherein.The sample powder that step S200 is obtained slowly is poured onto in mixing etching liquid（Added in magnetic agitation）To prevent
Bumping.Corrosion process continues 36 hours in the state of 40 DEG C of water-bath, and magnetic agitation is used in corrosion process.Etching process
Shown in reaction mechanism equation below：
Mn+1AlXn+3LiF+3HCl=AlF3+ Mn+1Xn+3LiCl+1.5H2 (4)
（4）Powder mixed liquor after etching processing is carried out to can obtain layered two dimension after carrying out washing treatment and drying process
Material MXene.Concrete operation step is to the disperse system after etching（Powder mixed liquor）Centrifuge washing is carried out, centrifugation rate is set
For 8500 turns/min, each 5min of centrifugation time, make to be washed with deionized, until solution ph is up to 5.After carrying out washing treatment
Obtained sample carries out 1 hour pre-freeze, is then transferred in vacuum freezing drying oven and is dried, is taken out after 18 hours, you can
Obtain stratiform two-dimensional material Ti2C。
Fig. 4 is that embodiment two prepares Ti2C SEM figures.As can be seen that after being up to 20h corrosion, Ti2AlC corrodes
There is space in preceding closely layer structure, and the particle of bulk has obtained good etching, almost institute under scanning electron microscope observation
Some samples have been etched, and illustrate that corrosion is carried out very thorough.The result of overall pattern and relevant report is basically identical, then
It is secondary to prove to realize to Ti by this method2C preparation.In addition, the Ti prepared by this method2C exists in the presence of some radiuses
1nm or so particle, these particles do not know its concrete component temporarily due to not obtaining embodying in XRD spectrum, but the shape
Looks obviously help increase Ti2The specific surface areas of C in itself, there should be castering action for the related property of its electrochemistry.
Fig. 5 is embodiment two（Using HCl＆LiF mixed solutions）The Ti2C of gained XRD spectrum analysis is performed etching, its
Diffraction maximum position substantially with embodiment one（HF）It is consistent to etch result.But at 13 ° of 2theta（002）Spread out corresponding to crystal face
Penetrate peak equally to be offset to less angle here, diffraction maximum is slightly widened.Corresponding to Al layers（104）Peak disappears, card
It is bright that Ti can also be prepared by this method2C.Comparatively, corrode to obtain Ti using HCl＆LiF mixed solutions2C characteristic peak
It is more sharp, illustrate the Ti of the preparation using this method2C crystallinity is preferable.This is probably due to the corrosion bar using HCl＆LiF
Part is comparatively gentle, smaller for bulk crystal structural damage compared with being corroded using HF.
Stratiform two-dimensional material Ti made from the present embodiment2C chemical property evaluation.
Weigh 0.0810g Ti2C sample, 0.0102g acetylene blacks and 0.0103g PVDF, it is fully mixed in agate mortar
It is even, add 1 mL ethanol and form grume material.Nickel foam is cut into the cm of 1 cm × 1 small pieces, in 3 M KOH solution
After 12 h of middle immersion, dry.8 mg grumes materials are equably applied to nickel foam small pieces side, pressed using 5 MPa
Piece.The electrode slice tests its specific capacity in three-electrode system, and electrolyte uses 3 M KOH solution.With potential window 0-0.5
V test loop VA characteristic curves, the specific capacity being converted to are used to assess the specific capacity that the invention prepares Ti2CTx：
The Ti of table 12Specific discharge capacity under C difference current densities
| Current density A/g | Specific discharge capacity F/g (HF) |
| 1 | 144.3 |
| 2 | 130.21 |
| 3 | 120.01 |
| 5 | 119.32 |
| 8 | 100.45 |
As seen from table, the Ti prepared using the method2C sample has preferable specific capacity property.
Embodiment three
The present embodiment prepares stratiform two-dimensional material Ti2C.Specific preparation process is as follows：
S100：Ternary material Ti is prepared using normal pressure-sintered technique2AlC.The step is identical with embodiment one.But it is normal pressure-sintered
Nitrogen protection is lower to be carried out.
S200：By normal pressure-sintered obtained ternary material Ti2AlC is ground into powder.
S300：Using HNO3Mixing KF performs etching processing to the powder, and the time of the etching processing is 50 hours.
The concrete operation step of etching processing is：Take the M HNO of 30 mL 63Solution, by 1.98 g KF（Analyze pure）Add
Enter to wherein.The sample powder that step S200 is obtained several times, is slowly added into mixing etching liquid, added on a small quantity every time
While magnetic agitation, to prevent bumping.Corrosion process continues 50 hours, made in corrosion process in the state of 40 DEG C of water-bath
Use magnetic agitation.Shown in the reaction mechanism equation below of etching process：
Mn+1AlXn+3KF+3HNO3=AlF3+ Mn+1Xn+3KNO3+1.5H2 (5)
（4）Powder mixed liquor after etching processing is carried out to can obtain layered two dimension after carrying out washing treatment and drying process
Material MXene.This step is the same as embodiment one.
Example IV
The present embodiment prepares stratiform two-dimensional material Nb2C.Specific preparation process is as follows：
S100：Ternary material Nb is prepared using normal pressure-sintered technique2AlC。
Wherein step S100 includes following operating procedure again：
S110：Weigh appropriate elemental powders Nb powder, pure Al powder and graphite powder；The Nb powder used in the present embodiment for (120 mesh,
Mass fraction 99.5%), pure Al powder is（200 mesh, mass fraction 99.7%）And graphite powder is（400 mesh, mass fraction
99.85%）.Concrete operations are to weigh 21.37 g Nb powder；The graphite powder of 3.57g pure Al powder and 1.38g, according to atomic ratio M：
A:X is 2:1.15:1.
S120：The a variety of elemental powders weighed are well mixed and carry out briquetting and handle to obtain briquetting.Pressed
Before block processing preferably by elemental powders using high speed ball mill by mixture ball milling 25h, the purpose for carrying out ball-milling treatment is
To evengranular mixed-powder.Briquetting processing in the present embodiment is with 10-20 MPa by mixed-powder using cuber
Pressure lower lock block is into 3 × 3 cm2 - 10×10 cm2Block.
S130：Normal pressure calcination processing is carried out to the briquetting and can obtain ternary material Nb2AlC.Specific operation process is
Briquetting is calcined using high temperature process furnances；Setting program is warming up to 1000-1700 DEG C, high temperature hold time 1-3h, forges
Whole process is burnt to carry out under vacuum conditions.
S200：By normal pressure-sintered obtained ternary material Nb2AlC is ground into powder.
S300：Processing is performed etching to the powder using HI mixing NaF, the time of the etching processing is 48 hours.
Shown in the reaction mechanism equation below of etching process：
Mn+1AlXn+3NaF+3HI=AlF3+ Mn+1Xn+3NaI+1.5H2 (6)
（4）Powder mixed liquor after etching processing is carried out to can obtain layered two dimension after carrying out washing treatment and drying process
Material MXene.Concrete operation step is to the disperse system after etching（Powder mixed liquor）Centrifuge washing is carried out, centrifugation rate is set
For 8500 turns/min, each 5min of centrifugation time, make to be washed with deionized, until solution ph is up to 5.After carrying out washing treatment
Obtained sample carries out 1.5 hours pre-freezes, is then transferred in vacuum freezing drying oven and is dried, is taken out after 20 hours, i.e.,
It can obtain stratiform two-dimensional material Nb2C。
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be defined by claim.
Claims (10)
1. a kind of stratiform two-dimensional material MXene preparation method, it is characterised in that comprise the following steps：
S100：Ternary material M is prepared using normal pressure-sintered techniquen+1AXn, wherein M is transition metal, and A is the 3rd or the 4th main group
Element, X are C or N element, n 1,2, or 3；
S200：By normal pressure-sintered obtained ternary material Mn+1AXnIt is ground into powder；
S300：Processing is performed etching to the powder, the time of the etching processing is 8 ~ 50 hours；
S400：Powder mixed liquor after etching processing is carried out to can obtain layered two after carrying out washing treatment and drying process
Tie up material MXene.
2. preparation method according to claim 1, it is characterised in that the step S100 specifically comprises the following steps：
S110：Weigh appropriate elemental powders；
S120：The a variety of elemental powders weighed are well mixed and carry out briquetting and handle to obtain briquetting；
S130：Normal pressure calcination processing is carried out to the briquetting and can obtain ternary material Mn+1AXn, wherein the normal pressure calcination processing
Temperature be 1000-1700 DEG C, calcination time be 0.8 ~ 5 hour.
3. preparation method according to claim 2, it is characterised in that the normal pressure calcination processing is in vacuum environment or nitrogen
Or carried out under the protection of inert gas.
4. preparation method according to claim 1, it is characterised in that the etching that etching processing described in step S300 uses
Agent is HF.
5. preparation method according to claim 1, it is characterised in that the etching agent of etching processing use is stated in step S300
For strong acid and the mixed solution of fluoride salt.
6. preparation method according to claim 5, it is characterised in that the strong acid be hydrochloric acid, sulfuric acid, nitric acid, perchloric acid,
One or more mixtures of selenic acid, hydrobromic acid, hydroiodic acid, chloric acid etc.；
And/or the fluoride is lithium fluoride, potassium fluoride, sodium fluoride, one or more mixtures of ammonium acid fluoride etc..
7. preparation method according to claim 1, it is characterised in that the carrying out washing treatment is centrifuge washing processing, to institute
The powder carrying out washing treatment after etching processing is stated until the pH value of solution is 4.5 ~ 5.6.
8. preparation method according to claim 1, it is characterised in that the drying process includes what is obtained afterwards to washing
Sample first carries out pre-freeze processing, and the sample is then dried into processing at 1000-1700 DEG C again.
9. according to the preparation method described in claim 1 to 8 any one, it is characterised in that the M is Ti, Nb or V, and A is
Al。
10. stratiform two dimension material made from the preparation method of the stratiform two-dimensional material MXene described in claim 1 to 9 any one
Expect applications of the MXene in energy storage, electrode and adsorbing domain.
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| CN110639569A (en) * | 2019-06-16 | 2020-01-03 | 浙江工业大学 | Unsaturated coordination-rich two-dimensional ceramic material catalyst and preparation method and application thereof |
| CN111732103A (en) * | 2020-06-10 | 2020-10-02 | 中国科学技术大学 | Fluorine-free Mo2CTx MXenes material, preparation method and application thereof |
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| CN113526506A (en) * | 2020-04-17 | 2021-10-22 | 北京化工大学 | Method for preparing TiO by adopting etching-ball milling method2/Ti3C2Method for compounding nano material |
| CN114076785A (en) * | 2020-08-11 | 2022-02-22 | 北京化工大学 | Sensor based on MXene/silk fibroin material and preparation method and application thereof |
| CN114335527A (en) * | 2020-09-29 | 2022-04-12 | 山东海科创新研究院有限公司 | High-performance silicon-carbon composite material, preparation method thereof and lithium ion battery |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699159A (en) * | 2005-04-29 | 2005-11-23 | 北京交通大学 | Titanium aluminium carbide powder and synthesis method using tin as reactive adjuvant therefor |
| CN101186294A (en) * | 2007-12-12 | 2008-05-28 | 哈尔滨工业大学 | Method of preparing high purity Ti2AlC block material |
| 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 |
| CN107001051A (en) * | 2014-09-25 | 2017-08-01 | 德雷塞尔大学 | Show the physical form of the MXene materials of new electrical and optical properties |
-
2017
- 2017-08-07 CN CN201710667543.2A patent/CN107522202A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699159A (en) * | 2005-04-29 | 2005-11-23 | 北京交通大学 | Titanium aluminium carbide powder and synthesis method using tin as reactive adjuvant therefor |
| CN101186294A (en) * | 2007-12-12 | 2008-05-28 | 哈尔滨工业大学 | Method of preparing high purity Ti2AlC block material |
| CN107001051A (en) * | 2014-09-25 | 2017-08-01 | 德雷塞尔大学 | Show the physical form of the MXene materials of new electrical and optical properties |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 郑伟 等: "二维纳米材料MXene的研究进展", 《材料导报A:综述篇》 * |
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| CN114335527B (en) * | 2020-09-29 | 2024-04-09 | 山东海科创新研究院有限公司 | High-performance silicon-carbon composite material, preparation method thereof and lithium ion battery |
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