CN110386602A - A kind of preparation method of titanium carbide/azepine graphene hydrogel photoelectric conversion material - Google Patents
A kind of preparation method of titanium carbide/azepine graphene hydrogel photoelectric conversion material Download PDFInfo
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- CN110386602A CN110386602A CN201910676868.6A CN201910676868A CN110386602A CN 110386602 A CN110386602 A CN 110386602A CN 201910676868 A CN201910676868 A CN 201910676868A CN 110386602 A CN110386602 A CN 110386602A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- 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
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of titanium carbide/azepine graphene hydrogel photoelectric conversion material preparation methods, comprising the following steps: (1) prepares Ti3C2；(2) it is spare to prepare graphite oxide suspension, weighs Ti obtained in step (1)3C2Into centrifuge tube, the graphite oxide solution of predetermined volume is then pipetted, is subsequently ultrasonicated for removal precipitating；(3) arginine is added in the solution that step (2) obtain, continues to be ultrasonically treated；(4) finally solution obtained above is transferred in vial and is reacted, after reaction, cleaned with pure water, obtain Ti3C2/ NGH nano heterojunction material.The present invention has the advantages such as preparation condition is mild, process is simple, and technique is controllable, and at low cost, large specific surface area, electric conductivity is good, and photoelectric conversion performance is good, is conducive to the application in fields such as lithium ion battery, fuel cell, solar batteries.
Description
Technical field
The invention belongs to functional nanocomposite preparation and its applied technical fields, and in particular to a kind of titanium carbide/nitrogen
Miscellaneous graphene hydrogel (Ti3C2/ NGH) photoelectric conversion material preparation method.
Background technique
Economic rapid growth not only brings global energy loss quickening and energy reserves deficiency problem, also unavoidably
Ground brings environmental problem.Therefore, there is an urgent need to excavate efficient, cleaning and sustainable new energy to alleviate the current energy
Crisis and problem of environmental pollution.Among the energy of many cleaning sustainable developments, solar energy is because it is easily obtained, can make repeatedly
With and environmental-friendly unique advantage play highly important role.Electric energy is from a wealth of sources and hold as a kind of secondary energy sources
Continuous cleaning uses if solar energy can be converted into electric energy by specific technology and be supplied to people, and solar energy will be a kind of reason
The alternative energy source thought.And the nano material of novel high-photoelectric transformation efficiency is studied and develops, and apply it on switching device
It is the important subject for meeting the demand.Single nano material as photo-electric conversion element its transfer efficiency often
It is not satisfactory, its suitable support material excellent with other performance is coupled be improve its photoelectric conversion performance effective way it
One.
MXenes is a kind of New Type of Carbon/nitride two-dimensional nano stratified material, began one's study and is developed so far from 2011,
Through the close attention for causing energy field scientific research personnel.So far, more than 20 kinds of MXenes materials are successfully made
It is standby.Titanium carbide (Ti3C2) receive scientific research personnel by the most wide feature of its search time longest, use scope and greatly favor.
However, being different from the high conductivity of carbon material, Ti3C2Intrinsic specific surface area is smaller, is easy the disadvantages of stacking, and leads to its electrification
Performance is learned to be substantially reduced.Research shows that by Ti3C2It couples to form novel composite material with good basis material, is to Ti3C2
One of effective means being modified.Currently, Ti3C2At home and abroad different field tentatively shows application to based composites
And researching value.
Azepine graphene hydrogel (NGH), also referred to as three-dimensional azepine graphene, is the three-dimensional based on azepine graphene
Porous material, have high mechanical strength, high-specific surface area, swift electron conducting power and extremely-low density, high porosity and solely
Special three-dimensional manometer characteristic, is a kind of Graphene derivative with good physical chemical property, obtains in electrochemistry
It is widely applied.The method for preparing azepine graphene hydrogel at present mainly has gel method, template and hydro-thermal method.
In the prior art, the photoelectric conversion material of Development of Novel is needed to improve the utilization efficiency of energy.Ti3C2As one
The emerging energy storage material of kind carries out further modification to it and has important practical significance.By the physical chemistry that NGH is excellent
Performance is combined with MXenes material performance outstanding in terms of the energy, it is contemplated that the utilization efficiency of energy can be effectively improved,
Develop new and effective photoelectric conversion material.
Summary of the invention
It is an object of the invention to overcome Ti in the prior art3C2Electric conductivity is poor, electron mobility is low, energy conversion effect
The low problem of rate provides and a kind of prepares Ti3C2The method of/NGH photoelectric conversion material.The material show good electric conductivity and
Photoelectric conversion efficiency.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of titanium carbide/azepine graphene hydrogel photoelectric conversion material, comprising the following steps:
(1) Ti is prepared3C2；
(2) it is spare to prepare graphite oxide suspension, weighs Ti obtained in step (1)3C2Into centrifuge tube, then pipette
The graphite oxide solution of predetermined volume is subsequently ultrasonicated for removal precipitating；
(3) arginine is added in the solution that step (2) obtain, continues to be ultrasonically treated；
(4) finally solution obtained above is transferred in vial and is reacted, after reaction, cleaned with pure water,
Obtain Ti3C2/ NGH nano heterojunction material；
Wherein, the Ti3AlC2Powder dosage is 2~10g；The concentration of the GO is 1.5~3mg/mL；The Ti3C2With
The mass ratio of the dosage of GO is 5~20:1；The arginic dosage is 100~300mg.
Further, the step (1) includes:
By Ti3AlC2Powder is distributed in HF acid solution, is stirred at room temperature to remove al atomic layer；
Then obtained powder is centrifuged repeatedly washing with deionized water several times, until the pH of dispersion liquid reaches 5~6；
Then the wet deposition object Ti of acquisition3C2TxIt is dried to obtain Ti3C2TxPowder；
Then by Ti3C2TxPowder is dispersed in ethyl alcohol, dimethylformamide and dimethyl sulfoxide, is ultrasonically treated；
Obtained dispersion liquid is kept into N2To remove oxygen in atmosphere, vacuum drying obtains Ti3C2Powder.
Further, the volume fraction of the HF acid solution is 49%；Wet deposition object Ti3C2TxDrying temperature and
The drying temperature of baking oven is 80 DEG C；Dispersion liquid is in N230min is kept in atmosphere.
Further, in the step (2) and (3), the time of the ultrasonic treatment is 8~10 minutes.
Further, in the step (4), vial is placed in reaction kettle and is put into electric drying oven with forced convection, 120
It is reacted 12 hours under the conditions of DEG C.
The invention has the following beneficial effects:
(1) the present invention provides a kind of Ti3C2The preparation method of/NGH photoelectric conversion material, the preparation method mild condition,
Method is simple, is very beneficial for industrialization；
(2) Ti prepared by the present invention3C2/ NGH nano heterojunction, compares single Ti3C2, electric conductivity and photoelectricity turn
It is transsexual to be obviously improved；
(3) present invention is successfully prepared Ti3C2Based nano composite material, and it is successfully used as photoelectric conversion material, it improves
Its energy utilization efficiency, has expanded its possible application field, can look forward to it in energy related field and possess preferable application
Prospect.
Detailed description of the invention
Fig. 1 is prepared Ti3C2The digital photograph under fluorescent light of/NGH；
Fig. 2 is X-ray diffraction (XRD) figure of prepared nanocomposite；
Fig. 3 is Ti3C2And Ti3C2The impedance spectrum of/NGH；
Fig. 4 is Ti3C2And Ti3C2The photoelectric conversion performance map of/NGH.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
A kind of preparation method of titanium carbide/azepine graphene hydrogel photoelectric conversion material of the present invention includes the following steps:
(1)Ti3C2Preparation:
Ti is prepared using hydrofluoric acid (HF) etching method3C2, detailed process is as follows: by Ti3AlC2Powder is distributed to volume fraction
To be stirred at room temperature and removing al atomic layer for 24 hours in 49%HF acid solution, then by obtained powder with deionized water several times repeatedly from
Heart washing achievees the purpose that completely remove residual HF and impurity until the pH of dispersion liquid reaches 5~6.Then the wet heavy of acquisition
Product object (Ti3C2Tx) dry 12h obtains Ti at 80 DEG C3C2TxPowder.Then by Ti3C2TxPowder is dispersed in ethyl alcohol, dimethyl
In formamide and dimethyl sulfoxide, (400W, 3h) is ultrasonically treated.Therewith, obtained dispersion liquid is kept into N2Atmosphere
30min removes oxygen, and setting baking oven is dried in vacuo at a temperature of 80 DEG C obtains Ti3C2Powder；
(2) Ti obtained in the step of preparation graphite oxide (GO) suspension first is spare, weighs certain mass (1)3C2Extremely
In centrifuge tube, the GO solution of certain volume is then pipetted, is subsequently ultrasonicated for the precipitating of removal in 8~10 minutes；
(3) it weighs a certain amount of arginine (nitrogen source) to be added in the solution that step (2) obtain, continues 8~10 points of ultrasonic treatment
Clock.
(4) finally solution obtained above is transferred in vial, and vial is placed in reaction kettle and is put into
In electric drying oven with forced convection, reacted 12 hours under the conditions of 120 DEG C.Reaction kettle is taken out after reaction, takes out vial, is changed pure
Water cleans several times, obtains Ti3C2/ NGH nano heterojunction material.
Wherein, the Ti3AlC2Powder dosage is 2~10g；The concentration of the GO is 1.5~3mg/mL；The Ti3C2With
The mass ratio of the dosage of GO is 5~20:1；The dosage of the arginine (nitrogen source) is 100~300 mg.
Embodiment 1
(1)Ti3C2Preparation:
Ti is prepared using hydrofluoric acid (HF) etching method3C2, detailed process is as follows: weighing 2gTi3AlC2Powder is distributed to volume
Score is to be stirred at room temperature in 49%HF acid solution and remove al atomic layer for 24 hours, then that obtained powder is anti-several times with deionized water
Multiple centrifuge washing achievees the purpose that completely remove residual HF and impurity until the pH of dispersion liquid reaches 5-6.Then, by acquisition
Wet deposition object (Ti3C2Tx) dry 12h obtains Ti under 80 °3C2TxPowder.Then, by Ti3C2TxPowder is dispersed in ethyl alcohol, two
In methylformamide and dimethyl sulfoxide, (400W, 3h) is ultrasonically treated.And then, obtained dispersion liquid is kept into N2
Atmosphere 30min is to remove oxygen.Finally, setting baking oven is dried in vacuo at a temperature of 80 ° and obtains Ti3C2Powder；
(2) Ti obtained in the step of compound concentration is that 1mg/mL GO suspension is spare first, weighs 5mg (1)3C2Powder
In centrifuge tube, the GO solution of 10mL is then pipetted, the extra sediment of ultrasound 8~remove after ten minutes in solution；
(3) it weighs 100mg arginine (nitrogen source) to be added in the solution that step (2) obtain, continues 8~10 points of ultrasonic treatment
Clock.
(4) finally solution obtained in above-mentioned steps (3) is transferred in vial, and vial is placed in and is reacted
It puts into electric drying oven with forced convection in kettle, is reacted 12 hours under the conditions of 120 DEG C.Reaction kettle is taken out after 12 hours, is changed ultrapure
Water cleans several times, obtains Ti3C2The nano heterogeneous material of/NGH.
Wherein, the Ti3AlC2Powder dosage is 2~10g；The concentration of the GO is 1.5~3mg/mL；The Ti3C2With
The mass ratio of the dosage of GO is 5~20:1；The dosage of the arginine (nitrogen source) is 100~300 mg.
Embodiment 2
(1)Ti3C2Preparation:
Ti is prepared using hydrofluoric acid (HF) etching method3C2, detailed process is as follows: weighing 5gTi3AlC2Powder is distributed to volume
Score is to be stirred at room temperature in 49%HF acid solution and remove al atomic layer for 24 hours, then that obtained powder is anti-several times with deionized water
Multiple centrifuge washing achievees the purpose that completely remove residual HF and impurity until the pH of dispersion liquid reaches 5~6.Then, it will obtain
Wet deposition object (Ti3C2Tx) dry 12h obtains Ti under 80 °3C2TxPowder.Then, by Ti3C2TxPowder be dispersed in ethyl alcohol,
In dimethylformamide and dimethyl sulfoxide, (400W, 3h) is ultrasonically treated.And then, obtained dispersion liquid is kept
N2Atmosphere 30min is to remove oxygen.Finally, setting baking oven is dried in vacuo at a temperature of 80 ° and obtains Ti3C2Powder；
(2) Ti obtained in the step of compound concentration is that 2mg/mL GO suspension is spare first, weighs 5mg (1)3C2Powder
In centrifuge tube, the GO solution of 10mL is then pipetted, the extra sediment of ultrasound 8~remove after ten minutes in solution；
(3) it weighs 200mg arginine (nitrogen source) to be added in the solution that step (2) obtain, continues 8~10 points of ultrasonic treatment
Clock.
(4) finally solution obtained in above-mentioned steps (3) is transferred in vial, and vial is placed in and is reacted
It puts into electric drying oven with forced convection in kettle, is reacted 12 hours under the conditions of 120 DEG C.Reaction kettle is taken out after 12 hours, is changed ultrapure
Water cleans several times, obtains Ti3C2/ NGH nano heterojunction material.By the macroscopical cylinder for being visually observed NGH carrier material
Structure, as shown in Figure 1.
Fig. 2 show the Ti prepared under the embodiment3C2And Ti3C2The X ray diffracting spectrum of/NGH, by with standard card
Piece comparison, discovery main diffraction peak coincide substantially, illustrate Ti3C2/ NGH nano heterojunction is successfully prepared；Fig. 3 is shown
The Ti prepared under the embodiment3C2And Ti3C2The impedance spectrum of/NGH, from the graph, it is apparent that resistance after nano material is compound
Half circular diameter of anti-map is obviously reduced, and shows Ti3C2It is substantially reduced with NGH composite impedance, electric conductivity is obviously improved；In order to
The prepared Ti of characterization3C2The photoelectric conversion performance of/NGH nano heterojunction material, to Ti3C2And Ti3C2/ NGH is having no light
Lower its photosignal response curve of acquisition, discovery and single Ti3C2It compares, Ti3C2The photo-signal of/NGH is obviously improved,
Illustrate prepared Ti3C2/ NGH nano heterojunction material has good photoelectric conversion performance.
Embodiment 3
(1)Ti3C2Preparation:
Ti is prepared using hydrofluoric acid (HF) etching method3C2, detailed process is as follows: weighing 10gTi3AlC2Powder is distributed to body
Fraction be 49%HF acid solution in, be stirred at room temperature and remove al atomic layer for 24 hours, then by obtained powder with deionized water several times
It is centrifuged repeatedly washing, until the pH of dispersion liquid reaches 5~6, achievees the purpose that completely remove residual HF and impurity.Then, it will obtain
Wet deposition object (the Ti obtained3C2Tx) dry 12h obtains Ti under 80 °3C2TxPowder.Then, by Ti3C2TxPowder is dispersed in second
In alcohol, dimethylformamide and dimethyl sulfoxide, it is ultrasonically treated (400W, 3h).And then, obtained dispersion liquid is protected
Hold N2Atmosphere 30min is to remove oxygen.Finally, setting baking oven is dried in vacuo at a temperature of 80 ° and obtains Ti3C2Powder；
(2) Ti obtained in the step of compound concentration is that 3mg/mL GO suspension is spare first, weighs 5mg (1)3C2Powder
In centrifuge tube, the GO solution of 10mL is then pipetted, the extra sediment of ultrasound 8~remove after ten minutes in solution；
(3) it weighs 300mg arginine (nitrogen source) to be added in the solution that step (2) obtain, continues 8~10 points of ultrasonic treatment
Clock.
(4) finally solution obtained in above-mentioned steps (3) is transferred in vial, and vial is placed in and is reacted
It puts into electric drying oven with forced convection in kettle, is reacted 12 hours under the conditions of 120 DEG C.Reaction kettle is taken out after 12 hours, is changed ultrapure
Water cleans several times, obtains Ti3C2/ NGH nano heterojunction material.
In conclusion the present invention provides a kind of hydro-thermal method self assemblies to prepare titanium carbide/azepine graphene hydrogel
(Ti3C2/ NGH) photoelectric conversion material method.The invention solves existing titanium carbide nano material electric conductivity, and poor, electronics moves
The problem that shifting rate is lower, photoelectric conversion efficiency is low.Method specifically includes: the first, the ternary layered Ti of high-purity3AlC2Powder warp
Hf etching removing, obtains the Ti of two-dimensional layer nano material MXene phase3C2Material；The second, hydro-thermal method makes to stablize in water phase
Existing graphite oxide (GO) self assembly realizes N doping, and and Ti with the nitrogen source arginine of addition3C2The functional group on surface into
Row effectively bonds together to form Ti3C2/ NGH nano heterojunction material.The present invention is mild with preparation condition, process is simple, and technique can
The advantages such as control, at low cost, large specific surface area, electric conductivity is good, and photoelectric conversion performance is good are conducive in lithium ion battery, combustion
Expect the application in the fields such as battery, solar battery.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention.It is all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (5)
1. a kind of titanium carbide/azepine graphene hydrogel photoelectric conversion material preparation method, comprising the following steps:
(1) Ti is prepared3C2；
(2) it is spare to prepare graphite oxide suspension, weighs Ti obtained in step (1)3C2Into centrifuge tube, then pipette predetermined
The graphite oxide solution of volume is subsequently ultrasonicated for removal precipitating；
(3) arginine is added in the solution that step (2) obtain, continues to be ultrasonically treated；
(4) finally solution obtained above is transferred in vial and is reacted, after reaction, cleaned, obtained with pure water
Ti3C2/ NGH nano heterojunction material；
Wherein, the Ti3AlC2Powder dosage is 2~10g；The concentration of the GO is 1.5~3mg/mL；The Ti3C2With GO's
The mass ratio of dosage is 5~20:1；The arginic dosage is 100~300mg.
2. a kind of titanium carbide according to claim 1/azepine graphene hydrogel photoelectric conversion material preparation method,
Be characterized in that: the step (1) includes:
By Ti3AlC2Powder is distributed in HF acid solution, is stirred at room temperature to remove al atomic layer；
Then obtained powder is centrifuged repeatedly washing with deionized water several times, until the pH of dispersion liquid reaches 5~6；
Then the wet deposition object Ti of acquisition3C2TxIt is dried to obtain Ti3C2TxPowder；
Then by Ti3C2TxPowder is dispersed in ethyl alcohol, dimethylformamide and dimethyl sulfoxide, is ultrasonically treated；
Obtained dispersion liquid is kept into N2To remove oxygen in atmosphere, vacuum drying obtains Ti3C2Powder.
3. a kind of titanium carbide according to claim 2/azepine graphene hydrogel photoelectric conversion material preparation method,
Be characterized in that: the volume fraction of the HF acid solution is 49%；Wet deposition object Ti3C2TxDrying temperature and baking oven drying
Temperature is 80 DEG C；Dispersion liquid is in N230min is kept in atmosphere.
4. a kind of titanium carbide according to claim 1/azepine graphene hydrogel photoelectric conversion material preparation method,
Be characterized in that: in the step (2) and (3), the time of the ultrasonic treatment is 8~10 minutes.
5. a kind of titanium carbide according to claim 1/azepine graphene hydrogel photoelectric conversion material preparation method,
It is characterized in that: in the step (4), vial being placed in reaction kettle and is put into electric drying oven with forced convection, it is anti-under the conditions of 120 DEG C
It answers 12 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113237933A (en) * | 2021-05-20 | 2021-08-10 | 常州工学院 | Titanium carbide modified bismuth heterophosphate photoelectrode and preparation method thereof |
| CN113979438A (en) * | 2021-12-23 | 2022-01-28 | 中博龙辉装备集团股份有限公司 | Graphene titanium carbide composite porous gel film and preparation method and application thereof |
-
2019
- 2019-07-25 CN CN201910676868.6A patent/CN110386602A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113237933A (en) * | 2021-05-20 | 2021-08-10 | 常州工学院 | Titanium carbide modified bismuth heterophosphate photoelectrode and preparation method thereof |
| CN113237933B (en) * | 2021-05-20 | 2022-11-04 | 常州工学院 | Titanium carbide modified bismuth heterophosphate photoelectrode and preparation method thereof |
| WO2022242095A1 (en) * | 2021-05-20 | 2022-11-24 | 常州工学院 | Titanium-carbide-modified bismuth-doped bismuth phosphate photoelectrode and preparation method therefor |
| CN113979438A (en) * | 2021-12-23 | 2022-01-28 | 中博龙辉装备集团股份有限公司 | Graphene titanium carbide composite porous gel film and preparation method and application thereof |
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