CN106981667A - A kind of preparation method of two-dimentional titanium carbide/carbon nanotube loaded platinum grain composite - Google Patents
A kind of preparation method of two-dimentional titanium carbide/carbon nanotube loaded platinum grain composite Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- H—ELECTRICITY
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- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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Abstract
The invention discloses a kind of preparation method of two-dimentional titanium carbide/carbon nanotube loaded platinum grain composite, comprise the following steps：Utilize HF chemical strippings Ti3AlC2In al atomic layer prepare two-dimentional titanium carbide；Solvent-thermal method causes two-dimentional titanium carbide to be combined with MWNTs, while the upper Pt nanoparticle of load, produces Ti3C2/ MWNTs Pt nano composite materials.Preparation method that the present invention is provided is simple, technique is controllable, reproducible, cost is low, beneficial to carrying out large-scale industrial production；And the Ti prepared3C2/ MWNTs Pt nano composite materials specific surface area is big, and electric conductivity is good, may be used as the anode catalyst of DMFC, excellent catalytic activity is gone out to methanol oxidation performance.
Description
Technical field
The invention belongs to nano composite material preparation field, more particularly to a kind of two-dimentional titanium carbide/carbon nanotube loaded
The preparation method of platinum grain composite.
Background technology
MXene is a kind of new two-dimentional class graphene transition metal carbide or carbonitride nanometer sheet, is to utilize HF
Selective etch falls what A atomic layers were obtained from ternary layered compound MAX, because it has the two-dimensional structure of similar graphene,
It is named as MXenes phase materials.Its chemical general formula is Mn+1XnTz, M is transiting group metal elements, and X is C and/or N element, T tables
What is shown is hydroxyl, oxonium ion or the fluorine ion isoreactivity functional group of its surface link, n=1,2 or 3.Presoma MAX phases belong to six
Prismatic crystal system, is the M by being alternately arrangedn+1XnLamella is formed by connecting with closelypacked A atomic layers, and M-X atom interlayers are mainly altogether
Valence link and ionic bond, M-A atoms interlayer is main to be connected with metallic bond, compared with M-X keys, and M-A bonds are weaker with joint efforts, so that
A layers of atomic reaction expression activitiy are high, it is easy to peel away.The MXene phases of current most study are Ti3C2, it is from corresponding using HF
MAX phases Ti3AlC2In separate what is obtained after Al atomic layers.The MXene for being prepared obtaining has bigger specific surface area and micro-
Interface, theoretical active and stability will be more preferable, for applied to anode catalysts for direct methanol fuel cell or ultracapacitor
Negative material provides possibility.
, can be with being rich in solution however, corroding obtained two-dimentional titanium carbide surface using HF contains exposed Ti atoms
F-、O2-Corresponding complex compound is formed with the functional groups such as OH-, steric hindrance is produced and electric conductivity is deteriorated.Meanwhile, actual system
It is difficult the MXene for separating individual layer or few layer during standby, specific surface area does not reach calculated value, and MXene surfaces can be compared with
Height, easy reunion caking causes dispersiveness poor, and the performance of its excellent properties is limited to a certain extent.Want preferably to apply
Two-dimentional titanium carbide, it is highly important research direction that surface modification and functionalization are carried out to it.Therefore, it is possible to a kind of by introducing
Low-dimensional materials with good conductivity, such as CNT, to reduce the reunion degree of titanium carbide, play both collaboration effects
Should, so as to improve the overall chemical property of material.
Carbon is very universal in nature, and the research and application of nano-carbon material are also quite varied.It is used as carbon material
Emerging member in family, CNT has started the research boom of a new round because of its unusual physical and chemical performance.Carbon is received
Mitron is a kind of structure carbon material of the 1-dimention nano size tubular found early 1990s, is a kind of seamless hollow pipe,
Formed by the curling of single or multiple lift graphene film, with performances such as many excellent mechanics, electricity, calorifics.In recent years with people
Nano materials research is goed deep into, the wide application prospect of CNT, application value are also constantly shown.
To sum up, the characteristic and novel energy-storing material based on two-dimentional titanium carbide are to the performance requirement of anode catalyst, HF corruption
Ti is prepared in erosion3C2Tx, and form Ti with multi-walled carbon nanotube (MWNTs) hydro-thermal reaction3C2/ MWNTs nano composite materials turn into
The precondition of catalytic reaction.Because the specific surface area of two-dimentional titanium carbide is larger, while MWNTs has excellent electric conductivity, electricity
Catalytic activity, can prevent the two-dimentional titanium carbide nanometer sheet of chemical stripping from reuniting again, and both are combined and is expected to give full play to two
The cooperative effect of person, can provide more active sites, contribute to the electro-chemical activity of reinforcing material, but specific property
Can be needed further further investigation, and the document report about MXene based composites is also less so far.
The content of the invention
Goal of the invention：Easily reunite for MXene phases titanium carbide material, the technological deficiency more than the number of plies, the present invention provides a kind of
Electric conductivity is good, catalytic activity is high and prepares the system of the low two-dimentional titanium carbide/carbon nanotube loaded platinum grain composite of cost
Preparation Method.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：A kind of two-dimentional titanium carbide/carbon nanotube loaded
The preparation method of platinum grain composite, comprises the following steps：
(1) by Ti3AlC2It is immersed in HF acid solutions, utilizes HF chemical strippings Ti3AlC2In al atomic layer, reacted
The reaction that may occur in journey has：
Ti3AlC2+ 3HF=AlF3+3/2H2+Ti3C2
Ti3C2+2H2O=Ti3C2(OH)2+H2
Ti3C2+ 2HF=Ti3C2F2+H2
Repeatedly centrifugation washing again after reaction terminates, obtains MXene phases Ti after drying3C2Powder.
(2) MWNTs is placed in condensing reflux in the mixed solution of concentrated nitric acid and the concentrated sulfuric acid, then repeatedly centrifugation washing, drying
The MWNTs that acidification is crossed is obtained afterwards.
(3) Ti for obtaining step (1)3C2Powder and the MWNTs for obtaining step (2) mixed-powder are by a certain percentage
The in the mixed solvent of ethylene glycol and deionized water is scattered in, while adding K2PtCl4, ultrasonic disperse, through hydrothermal synthesis reaction kettle height
Warm reaction under high pressure, then repeatedly centrifugation washing, obtain Ti after drying3C2/ MWNTs-Pt nano composite materials.
Preferably, in step (1), Ti3AlC2The sieve with 400 mesh is needed before powder corrosion, particle diameter is obtained and is less than 38 μm
Ti3AlC2Powder.
In step (1), described Ti3AlC2Reaction condition with HF is：HF concentration is 30~60wt%, it is therefore preferable to 40
~50%, reaction environment temperature is at 25~60 DEG C, and the reaction time is 20~60h.
In step (1), the centrifugal condition of two-dimentional titanium carbide is 3000~6000rpm, and 5~15min is centrifuged every time, if centrifugation
Dry time, until the pH value of last time centrifugation gained supernatant is controlled 6~7；In step (2), centrifugal condition be 5000~
10000rpm, centrifuges 5~30min every time, and the pH value to last time centrifugation gained supernatant is controlled 6~7；In step (3),
Centrifugal condition is 3000~6000rpm, and 5~30min is centrifuged every time, and the pH value control to last time centrifugation gained supernatant exists
6~7.
In step (2), the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3: 0.5~1.5.
In step (2), mixed solution is 2~8h of condensing reflux at 100~160 DEG C.
In step (3), wherein Ti3C2Mass ratio with MWNTs is 0.2~4.0, the volume ratio of ethylene glycol and deionized water
For 1: 0.5~1.5.The ultrasonic time of dispersion liquid is 0.5~2h.
In step (3), the condition of hydro-thermal reaction is 10~30h of reaction at 100~180 DEG C.
Preferably, K2PtCl4With Ti3C 2 Mass ratio be 1~5: 5~15.
In one embodiment, two-dimentional titanium carbide/carbon nanotube loaded platinum grain composite wood is made by the steps
Material：
(1) by 0.2~1.5gTi3AlC2Powder is immersed in 30~60%HF acid solutions, utilizes the sour chemical strippings of HF
Ti3AlC2In al atomic layer, be then centrifuged for washing, after drying MXene phases Ti3C2Powder；
(2) 50~120mg MWNTs are placed in the mixed solution of 50~120mL concentrated nitric acids and the concentrated sulfuric acid, wherein dense nitre
The volume ratio of acid and the concentrated sulfuric acid is 3: 0.5~1.5, condensing reflux, then centrifuges washing, and the MWNTs that acidification is crossed is obtained after drying；
(3) Ti for obtaining 5~15mg steps (1)3C2The MWNTs powder obtained with step (2) mixes (Ti used3C2With
The quality of MWNTs mixed-powders is 10~30mg) in the mixed solvent of 50~150mL ethylene glycol and deionized water is scattered in, its
Middle Ti3C2Mass ratio with MWNTs is 0: 10~10: 0, and the volume ratio of ethylene glycol and deionized water is 1: 0.5~1.5, while plus
Enter 1~5mg K2PtCl4, ultrasonic disperse, through hydrothermal synthesis reaction kettle high-temperature high-voltage reaction, then repeatedly centrifugation washing, after drying
Obtain Ti3C2/ MWNTs-Pt nano composite materials.
Beneficial effect：Easily reunite for two-dimentional titanium carbide, the number of plies is more, specific surface area and electric conductivity can not reach theoretical calculation
The defect of value, is answered the invention provides a kind of two-dimentional titanium carbide/carbon nanotube loaded platinum grain of the high preparation of simple to operate, quality
The method of condensation material.The present invention is with Ti3AlC2For raw material, al atomic layer is peeled off by HF and obtains two-dimentional titanium carbide, then using solvent
Hot method causes two-dimentional titanium carbide to be combined with MWNTs, while the upper Pt nanoparticle of load, obtains Ti3C2/ MWNTs-Pt nanometers multiple
Condensation material.Preparation method that the present invention is provided is simple, technique is controllable, reproducible, cost is low, beneficial to carrying out large-scale industry life
Production；And the Ti prepared3C2/ MWNTs-Pt nano composite materials specific surface area is big, and electric conductivity is good, may be used as directly
The anode catalyst of methanol fuel cell, excellent catalytic activity is gone out to methanol oxidation performance.
Brief description of the drawings
Fig. 1 is Ti prepared by embodiment 13C2There is the diffraction maximum of each component on/MWNTs-Pt XRD spectrum, figure, this table
Bright three component is successfully combined with each other；
Fig. 2 is the Ti that obtains in embodiment 13C2/ MWNTs-Pt SEM shape appearance figures, MWNTs and Ti3C2It is cross-linked with each other and twines
Around part MWNTs has been successfully plugged into Ti3C2Interlayer, it is possible to increase the contact area of catalyst, is conducive to ion transport, so as to carry
The overall electro catalytic activity of high material；
Fig. 3 is Ti in embodiment 13C2/ MWNTs-Pt electro-chemical test performance map, a figures are the composites in 1M
H2SO4In cyclic voltammetry curve figure, by suction/desorption peak area of hydrogen during negative electricity bit scan can calculate electrochemistry live
Property surface area (ECSA), is 154m2/g；B figures are the samples in 1M H2SO4+2MCH3Cyclic voltammetry curve in OH electrolyte
Figure, two peak currents are occurred in that in 0.7 and 0.5V region, correspond respectively to the electrochemical oxidation peak of methanol and middle poisoning production
Thing CO oxidation peak, peak current is larger, and preferable electro catalytic activity is gone out to methanol oxidation performance.
Embodiment
The present invention is described in detail below by specific embodiment.
Embodiment 1
By 0.3g Ti3AlC2Powder (sieved with 400 mesh sieve, Ti3AlC2Particle diameter is less than 38 μm) in immersion at 25 DEG C
Into 20mL40%HF acid solutions, reaction 24h obtains suspension.Washing is repeatedly centrifuged to obtained suspension, centrifugal condition is
4000rpm, centrifuges 5min, and to the last once the pH value of centrifugation gained supernatant is close neutral.Obtained precipitated product is put
In in vacuum drying chamber, MXene phases Ti is obtained after 60 DEG C of drying3C2Powder.100mg MWNTs are taken to be placed in 100mL concentrated nitric acids and dense sulphur
In the mixed solution of acid, condensing reflux 3h at 100 DEG C, the wherein volume ratio of the concentrated sulfuric acid and concentrated nitric acid are 3: 1.By gained suspension
Repeatedly centrifugation washing, centrifugal condition is 8000rpm, centrifuges 10min, and to the last once the pH value of centrifugation gained supernatant is approached
It is neutral.Obtained precipitated product is placed in vacuum drying chamber, the MWNTs that acidification is crossed is obtained after 100 DEG C of drying.Again by 10mg
Ti3C2The mixing that the mixed-powder for the 10mg MWNTs that powder is crossed with acidification is scattered in 80mL ethylene glycol and deionized water is molten
In agent, wherein the volume ratio of ethylene glycol and deionized water is 1: 1, while adding 10mg K2PtCl4, ultrasonic disperse 1h.Ultrasound knot
Solution is placed in hydrothermal synthesis reaction kettle after beam, 16h is reacted at 100 DEG C and obtains precipitated product.To product under 4000rpm from
Heart 5min, repeatedly centrifugation is washed to the pH value for centrifuging gained supernatant for the last time close to neutrality, then is placed in 60 in vacuum drying oven
DEG C drying after Ti3C2/ MWNTs-Pt nano composite materials.Obtained Ti3C2/ MWNTs-Pt XRD spectrum is as shown in figure 1, figure
On have the diffraction maximum of each component, this shows that three components are successfully combined with each other.
Embodiment 2
By 0.3g Ti3AlC2Powder (sieved with 400 mesh sieve, Ti3AlC2Particle diameter is less than 38 μm) in immersion at 25 DEG C
Into 20mL40%HF acid solutions, reaction 48h obtains suspension.Washing is repeatedly centrifuged to obtained suspension, centrifugal condition is
5000rpm, centrifuges 5min, and to the last once the pH value of centrifugation gained supernatant is close neutral.Obtained precipitated product is put
In in vacuum drying chamber, MXene phases Ti is obtained after 80 DEG C of drying3C2Powder.80mg MWNTs are taken to be placed in 100mL concentrated nitric acids and dense sulphur
In the mixed solution of acid, condensing reflux 4h at 100 DEG C, the wherein volume ratio of the concentrated sulfuric acid and concentrated nitric acid are 3: 1.By gained suspension
Repeatedly centrifugation washing, centrifugal condition is 8000rpm, centrifuges 10min, and to the last once the pH value of centrifugation gained supernatant is approached
It is neutral.Obtained precipitated product is placed in vacuum drying chamber, the MWNTs that acidification is crossed is obtained after 100 DEG C of drying.Again by 12mg
Ti3C2The mixed-powder for the 8mg MWNTs that powder is crossed with acidification is scattered in 80mL ethylene glycol and the mixed solvent of deionized water
In, wherein the volume ratio of ethylene glycol and deionized water is 1: 1, while adding 6mg K2PtCl4, ultrasonic disperse 0.5h.Ultrasound terminates
Solution is placed in hydrothermal synthesis reaction kettle afterwards, 12h is reacted at 120 DEG C and obtains precipitated product.Product is centrifuged under 5000rpm
5min, repeatedly centrifugation is washed to the pH value for centrifuging gained supernatant for the last time close to neutrality, then is placed in vacuum drying oven 80 DEG C
Ti is obtained after drying3C2/ MWNTs-Pt nano composite materials.Gained Ti3C2/ MWNTs-Pt SEM shape appearance figures as shown in Fig. 2
MWNTs and Ti3C2Be cross-linked with each other winding, and part MWNTs has been successfully plugged into Ti3C2Interlayer, it is possible to increase the contact surface of catalyst
Product, is conducive to ion transport, so as to improve the overall electro catalytic activity of material.
Embodiment 3
By 0.3g Ti3AlC2Powder (sieved with 400 mesh sieve, Ti3AlC2Particle diameter is less than 38 μm) in immersion at 40 DEG C
Into 15mL 40%HF acid solutions, reaction 24h obtains suspension.Washing is repeatedly centrifuged to obtained suspension, centrifugal condition is
4000rpm, centrifuges 5min, and to the last once the pH value of centrifugation gained supernatant is close neutral.Obtained precipitated product is put
In in vacuum drying chamber, MXene phases Ti is obtained after 80 DEG C of drying3C2Powder.50mg MWNTs are taken to be placed in 80mL concentrated nitric acids and the concentrated sulfuric acid
Mixed solution in, condensing reflux 2.5h at 110 DEG C, the wherein volume ratio of the concentrated sulfuric acid and concentrated nitric acid be 3: 1.By gained suspension
Repeatedly centrifugation washing, centrifugal condition is 8000rpm, centrifuges 10min, and to the last once the pH value of centrifugation gained supernatant is approached
It is neutral.Obtained precipitated product is placed in vacuum drying chamber, the MWNTs that acidification is crossed is obtained after 100 DEG C of drying.Again by 8mg
Ti3C2The mixing that the mixed-powder for the 12mg MWNTs that powder is crossed with acidification is scattered in 80mL ethylene glycol and deionized water is molten
In agent, wherein the volume ratio of ethylene glycol and deionized water is 1: 1, while adding 12mg K2PtCl4, ultrasonic disperse 1h.Ultrasound knot
Solution is placed in hydrothermal synthesis reaction kettle after beam, 18h is reacted at 100 DEG C and obtains precipitated product.To product under 4000rpm from
Heart 5min, repeatedly centrifugation is washed to the pH value for centrifuging gained supernatant for the last time close to neutrality, then is placed in 80 in vacuum drying oven
DEG C drying after Ti3C2/ MWNTs-Pt nano composite materials.Fig. 3 is Ti in the embodiment3C2/ MWNTs-Pt electro-chemical test
Performance map, has surveyed the composite in 1M H2SO4In cyclic voltammetry curve figure, can be calculated using the area at hydrogen desorption peak
Electrochemical surface area, is 154m2/ g, shows preferable electro catalytic activity.
Embodiment 4
By 0.3g Ti3AlC2Powder (sieved with 400 mesh sieve, Ti3AlC2Particle diameter is less than 38 μm) in immersion at 50 DEG C
Into 10mL 50%HF acid solutions, reaction 12h obtains suspension.Washing is repeatedly centrifuged to obtained suspension, centrifugal condition is
5000rpm, centrifuges 5min, and to the last once the pH value of centrifugation gained supernatant is close neutral.Obtained precipitated product is put
In in vacuum drying chamber, MXene phases Ti is obtained after 60 DEG C of drying3C2Powder.80mg MWNTs are taken to be placed in 80mL concentrated nitric acids and the concentrated sulfuric acid
Mixed solution in, condensing reflux 2.5h at 120 DEG C, the wherein volume ratio of the concentrated sulfuric acid and concentrated nitric acid be 3: 1.By gained suspension
Repeatedly centrifugation washing, centrifugal condition is 8000rpm, centrifuges 15min, and to the last once the pH value of centrifugation gained supernatant is approached
It is neutral.Obtained precipitated product is placed in vacuum drying chamber, the MWNTs that acidification is crossed is obtained after 110 DEG C of drying.Again will
16mgTi3C2The mixed-powder for the 4mg MWNTs that powder is crossed with acidification is scattered in the mixing of 80mL ethylene glycol and deionized water
In solvent, wherein the volume ratio of ethylene glycol and deionized water is 1: 1, while adding 10mg K2PtCl4, ultrasonic disperse 1h.Ultrasound
Solution is placed in hydrothermal synthesis reaction kettle after end, 16h is reacted at 100 DEG C and obtains precipitated product.To product under 4000rpm
5min is centrifuged, repeatedly centrifugation is washed to the pH value for centrifuging gained supernatant for the last time close to neutrality, then is placed in vacuum drying oven
Ti is obtained after 60 DEG C of drying3C2/ MWNTs-Pt nano composite materials.
Embodiment 5
By 0.3g Ti3AlC2Powder (sieved with 400 mesh sieve, Ti3AlC2Particle diameter is less than 38 μm) in immersion at 25 DEG C
Into 20mL 40%HF acid solutions, reaction 24h obtains suspension.Washing is repeatedly centrifuged to obtained suspension, centrifugal condition is
5000rpm, centrifuges 5min, and to the last once the pH value of centrifugation gained supernatant is close neutral.Obtained precipitated product is put
In in vacuum drying chamber, MXene phases Ti is obtained after 60 DEG C of drying3C2Powder.100mg MWNTs are taken to be placed in 100mL concentrated nitric acids and dense sulphur
In the mixed solution of acid, condensing reflux 3h at 100 DEG C, the wherein volume ratio of the concentrated sulfuric acid and concentrated nitric acid are 3: 1.By gained suspension
Repeatedly centrifugation washing, centrifugal condition is 8000rpm, centrifuges 10min, and to the last once the pH value of centrifugation gained supernatant is approached
It is neutral.Obtained precipitated product is placed in vacuum drying chamber, the MWNTs that acidification is crossed is obtained after 100 DEG C of drying.Again by 14mg
Ti3C2The mixed-powder for the 6mg MWNTs that powder is crossed with acidification is scattered in 80mL ethylene glycol and the mixed solvent of deionized water
In, wherein the volume ratio of ethylene glycol and deionized water is 1: 1, while adding 12mg K2PtCl4, ultrasonic disperse 1h.Ultrasound terminates
Solution is placed in hydrothermal synthesis reaction kettle afterwards, 20h is reacted at 100 DEG C and obtains precipitated product.Product is centrifuged under 5000rpm
5min, repeatedly centrifugation is washed to the pH value for centrifuging gained supernatant for the last time close to neutrality, then is placed in vacuum drying oven 60 DEG C
Ti is obtained after drying3C2/ MWNTs-Pt nano composite materials.
Tables 1 and 2 is respectively the ECSA values that 5 embodiments are calculated and known some comparative samples (RGO/Pt, GNP/
Pt ECSA values).Electrochemical active surface has reacted the quantity in catalyst surface active site, thus is to weigh catalytic performance
An important indicator.Calculate and find, the ECSA values for the sample that we prepare are higher, hence it is evident that better than other carbon-based platinum composite woods
Material.
Table 1
Table 2
Claims (10)
1. the preparation method of a kind of two-dimentional titanium carbide/carbon nanotube loaded platinum grain composite, it is characterised in that including as follows
Step：
(1) by Ti3AlC2Powder is immersed in HF acid solutions, utilizes the sour chemical stripping Ti of HF3AlC2In al atomic layer, Ran Houli
Edema with the heart involved is washed, and MXene phases Ti is obtained after drying3C2Powder；
(2) MWNTs is placed in the mixed solution of concentrated nitric acid and the concentrated sulfuric acid, condensing reflux, then centrifuges washing, must be acidified after drying
Treated MWNTs；
(3) Ti for obtaining step (1)3C2The MWNTs powder obtained with step (2), which is mixed, is scattered in ethylene glycol and deionized water
In the mixed solvent, while add K2PtCl4, ultrasonic disperse, through hydrothermal synthesis reaction kettle high-temperature high-voltage reaction, then repeatedly centrifugation
Washing, obtains Ti after drying3C2/ MWNTs-Pt nano composite materials.
2. preparation method according to claim 1, it is characterised in that in step (1), Ti3AlC2Need to use before powder corrosion
400 mesh sieve are sieved, and obtain the Ti that particle diameter is less than 38 μm3AlC2Powder.
3. preparation method according to claim 1, it is characterised in that in step (1), described Ti3AlC2With HF reaction
Condition is：HF concentration is 30~60wt%, and reaction environment temperature is at 25~60 DEG C, and the reaction time is 20~60h.
4. preparation method according to claim 1, it is characterised in that in step (1), the centrifugal condition of two-dimentional titanium carbide is
3000~6000rpm, centrifuges 5~15min every time, centrifuges several times, until the pH value control of last time centrifugation gained supernatant
System is 6~7；In step (2), centrifugal condition is 5000~10000rpm, and 5~30min is centrifuged every time, and institute is centrifuged to last time
The pH value for obtaining supernatant is controlled 6~7；In step (3), centrifugal condition is 3000~6000rpm, and 5~30min is centrifuged every time,
PH value to last time centrifugation gained supernatant is controlled 6~7.
5. preparation method according to claim 1, it is characterised in that in step (2), the volume ratio of the concentrated sulfuric acid and concentrated nitric acid
For 3: 0.5~1.5.
6. preparation method according to claim 1, it is characterised in that in step (2), mixed solution is at 100~160 DEG C
2~8h of lower condensing reflux.
7. preparation method according to claim 1, it is characterised in that wherein Ti3C2With MWNTs mass ratio for 0.2~
4.0, the volume ratio of ethylene glycol and deionized water is 1: 0.5~1.5.
8. preparation method according to claim 1, it is characterised in that in step (3), time of ultrasonic disperse for 0.5~
2h。
9. preparation method according to claim 1, it is characterised in that in step (3), the condition of hydrothermal synthesis reaction is
10~30h is reacted at 100~180 DEG C.
10. preparation method according to claim 1, it is characterised in that K2PtCl4With Ti3C2Mass ratio for 1~5: 5~
15。
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| CN108398469A (en) * | 2018-03-27 | 2018-08-14 | 西南大学 | A kind of preparation method of novel titanium carbide/palladium/platinum nanocomposite |
| CN108641779A (en) * | 2018-04-25 | 2018-10-12 | 青岛大学 | A kind of TiO2Nano particle coats the preparation method of carbon-coating electric current change composite material |
| CN108855166A (en) * | 2018-06-20 | 2018-11-23 | 郑州轻工业学院 | A kind of loaded catalyst and preparation method thereof, application |
| CN109406611A (en) * | 2018-11-09 | 2019-03-01 | 武汉工程大学 | A kind of Technique of Nano Pd/carbon nanotube-MXene composite material and its application in nitro arene explosive substance detection |
| CN109449405A (en) * | 2018-10-30 | 2019-03-08 | 肇庆市华师大光电产业研究院 | A kind of sulphur-oxygen doping MXene- carbon nano tube compound material and its application in lithium-sulfur cell |
| 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 |
| CN109686936A (en) * | 2018-12-17 | 2019-04-26 | 深圳先进技术研究院 | Calcium ion battery cathode active material, negative electrode material, calcium ion battery cathode, calcium ion battery and its preparation method and application |
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| CN112310417A (en) * | 2020-11-05 | 2021-02-02 | 中国科学院合肥物质科学研究院 | Preparation method, product and application of three-dimensional platinum/Mxene-reduced graphene oxide catalyst |
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| CN110042424B (en) * | 2019-05-29 | 2021-04-13 | 辽宁大学 | Composite catalyst MXene/CNTs and preparation method and application thereof |
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| CN112310417A (en) * | 2020-11-05 | 2021-02-02 | 中国科学院合肥物质科学研究院 | Preparation method, product and application of three-dimensional platinum/Mxene-reduced graphene oxide catalyst |
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| CN113422077A (en) * | 2021-06-22 | 2021-09-21 | 合肥工业大学 | CO-resistant MXene-based catalyst for proton exchange membrane fuel cell and preparation method thereof |
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| CN117504750A (en) * | 2024-01-04 | 2024-02-06 | 中国科学院合肥物质科学研究院 | Low Pt-loaded MXene-carbon nanotube aerogel film, and preparation method and application thereof |
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