CN107099054A - Ti3C2The preparation method of MXene/ polymer composite wave-suction materials - Google Patents
Ti3C2The preparation method of MXene/ polymer composite wave-suction materials Download PDFInfo
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- CN107099054A CN107099054A CN201710334294.5A CN201710334294A CN107099054A CN 107099054 A CN107099054 A CN 107099054A CN 201710334294 A CN201710334294 A CN 201710334294A CN 107099054 A CN107099054 A CN 107099054A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a kind of Ti3C2The preparation method of MXene/ polymer composite wave-suction materials, it has just prepared efficient Ti using solution etches and compound method3C2MXene/ polymer composite wave-suction materials；Ti prepared by the present invention3C2MXene/ polymer composite wave-suction materials, not only density is light, intensity is high, dielectric constant is adjustable for the composite of formation, is more seldom, and composite has the absorption and reflection to electromagnetic wave, the secondary pollution it reduce electromagnetic wave to environment concurrently.Ti prepared by the present invention3C2MXene/ polymer composite wave-suction materials have the characteristics of light weight, thickness of thin, intensity are high, absorbing property is good, are with a wide range of applications.
Description
Technical field
The present invention relates to chemical material field, more particularly to a kind of Ti3C2MXene/ polymer composite wave-suction materials
Preparation method.
Background technology
The progress of science and technology so that electromagnetic technique creates huge material progress to the mankind, but people are also brought into one
In environment full of artificial electromagnetic radiation.Electromagnetic radiation pollution is had become after atmosphere pollution, water pollution and noise pollution
The 4th pollution sources, and with electronics, telecommunication technology is fast-developing and is on the rise.Civilian aspect, the transmitting of great-power electromagnetic ripple
The electromagnetic wave that tower, radio station etc. are outwardly constantly launched, the problems such as usually bringing communication interference, electronics dense fog.Even more serious
It is that millions of people are due to being chronically exposed in the electromagnetic radiation from cable and household appliances, cancer stricken and degeneration
Property disease danger increasing, frequency electromagnetic waves are to biological body cell, nerve system of human body, the circulatory system, immune, reproduction
There is extremely strong radiation injury with metabolic function.The method of conventional electromagnetic shielding can bring the high reflection of electromagnetic wave, therefore
Finding the material of low reflection high-selenium corn turns into the study hotspot of absorbing material.
Absorbing material refers to that the electromagnetic wave energy for projecting its surface, and the dielectric loss electromagnetic wave for passing through material can be absorbed
Energy is converted to heat energy or the energy of other forms.Traditional absorbing material mainly include carbon fiber, graphite, conduction high polymer,
Barium titanate, ferrite and metal fine powder etc..But traditional absorbing material wave absorbing agent content is high, not only increases the density of material
Also improve cost；Low, poor and traditional with the matching of the wave absorption base material suction ripple material of traditional absorbing material wave absorbing agent performance
The problem of material has high emission, not only overall absorbing property is low, but also can cause secondary pollution of the battery ripple to environment.
MXene is a kind of transition metal carbide with two-dimensional layered structure similar to graphene that be finding in recent years
Or nitride, a total of nearly 70 kinds, including Ti3C2, Ti2C, V2C, Nb2C, Nb4C3, Ta4C3 of the MXene having now been found that,
Ti4N3 etc..MXene is due to its good electric conductivity, big specific surface area and high intensity, in energy storage, electronics, composite wood
The fields such as material, sensor are with a wide range of applications.But simple MXene poor mechanical properties, greatly, cost is high for density, and
It is difficult to be attached in substrate.
Therefore, the prior art is defective, it is necessary to improve.
The content of the invention
The technical problems to be solved by the invention are：There is provided a kind of with light weight, thickness of thin, intensity height, absorbing property
Good Ti3C2The preparation method of MXene/ polymer composite wave-suction materials.
Technical scheme is as follows：A kind of Ti3C2The preparation method of MXene/ polymer composite wave-suction materials, S1：
Ti3C2MXene preparation；S11：Quantitatively weigh the Ti of MAX phases3AlC2, it is dissolved in the HF that concentration is 50%, is stirring it
Mix lower reaction 18-24h；S12：After the reaction solution filtering in step S11 and massive laundering solid, then in the case where 40 degree -60 is spent
Drying, that is, obtain Ti3C2MXene powder；S2：Ti3C2The preparation of/thin polymer film；S21:Quantitatively weigh Ti3C2MXene powder,
And be dissolved in dimethyl sulfoxide solution, the ultrasound 15-30min under 100w-300w；S22:By the Ti in step S213C2MXene solution
With mixed with polymers, 1-2h is stirred；Wherein, Ti3C2The mass ratio of MXene and polymer is 1：9-9：1；S23:Will
Ti3C2MXene polymer solutions are in 100w ultrasounds 0.5-1h；S24:By Ti3C2MXene polymer solutions are in 2000-3000rpm
Lower centrifugation 15min-30min；And obtained solid powder is dried into 24h under 40-60 degree, obtain Ti3C2MXene/ polymer is answered
Close powder；S25:By Ti3C2MXene/ polymer compound powder powder materials are dissolved in water and Ti are made later3C2MXene/ thin polymer films.
Applied to each above-mentioned technical proposal, in described preparation method, in step S25：By Ti3C2MXene/ polymer
Composite powder material is dissolved in after water, then obtains Ti by filtering or spin coating3C2MXene2/ thin polymer film.
Applied to above-mentioned technical proposal, in described preparation method, in step S22：Polymer be PVA or PMMA or
PVDF or PEI or PS.
Applied to each above-mentioned technical proposal, in described preparation method, in step S22：Ti3C2MXene and polymer
Mass ratio is 1：1.
Applied to each above-mentioned technical proposal, in described preparation method, in step S11：Quantitatively weigh MAX phases
Ti3AlC2For in 1g, also, step S21：Quantitatively weigh Ti3C2MXene powder is 1g.
Using such scheme, solution etches are only used only in the present invention and compound method has just been prepared efficiently
Ti3C2MXene/ polymer composite wave-suction materials, (oxidation is also for the more traditional two-dimensional material-graphene of preparation technology, molybdenum disulfide
Former, CVD) etc. greatly simplify, Ti prepared by the present invention3C2MXene/ polymer composite wave-suction materials, the composite of formation is not only
Density is light, intensity is high, dielectric constant is adjustable, is more seldom, and composite has the absorption and reflection to electromagnetic wave concurrently, this reduction
Secondary pollution of the electromagnetic wave to environment.Ti prepared by the present invention3C2MXene/ polymer composite wave-suction materials have light weight,
The characteristics of thickness of thin, intensity are high, absorbing property is good, is with a wide range of applications.
Brief description of the drawings
Fig. 1 a are Ti3C2MXene surface sweeping sem image figure；
Fig. 1 b are Ti3C2MXene/PVA scanning electron microscope image figure；
Fig. 2 is Ti3C2MXene and Ti3C2The curve map of MXene/PVA XRD picture；
Fig. 3 a are Ti3C2The curve map of MXene Raman image；
Fig. 3 b are Ti3C2The curve map of MXene/PVA Raman image；
Fig. 4 is Ti3C2The stress strain curve figure of MXene/PVA composite film materials；
Fig. 5 is the Ti of different-thickness3C2The suction ripple effect test result curve figure of MXene/PVA composites.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Present embodiments provide a kind of Ti3C2The preparation method of MXene/ polymer composite wave-suction materials, including following step
Suddenly：
First：Ti3C2MXene preparation
1) Ti of 1g MAX phases is weighed3AlC2, and be dissolved in the HF that concentration is 50%, 18-24h is reacted under agitation；
2) by above step 1) reaction solution filtering, massive laundering solid, and dry and obtain under 40 degree -60 degree again
Ti3C2MXene powder.
Then：Ti3C2The preparation of MXene/ thin polymer films
1) 1g Ti are weighed3C2MXene powder is dissolved in dimethyl sulfoxide solution, the ultrasound 15-30min under 100w-300w；
2) by above step 1) in Ti3C2MXene solution and mixed with polymers, stir 1-2h；Wherein, polymer bag
Include PVA, PMMA, PVDF, PEI, PS etc.；Also, Ti3C2The mass ratio of MXene and polymer is 1：9-9：1, wherein, preferably
For 1：1；
3) by Ti3C2MXene polymer solutions are in 100w ultrasounds 0.5-1h；
4) by above step 3) in by Ti3C2MXene polymer solutions centrifuge 15min-30min under 2000-3000rpm；
Obtained solid powder dries 24h under 40-60 degree, obtains Ti3C2MXene/ polymer compound powders；
5) by Ti3C2MXene/ polymer compound powder powder materials are dissolved in after water, are obtained by methods such as filtering, spin coatings
Ti3C2MXene/ thin polymer films.
Product of the present invention will use laser Raman spectrometer (laser Raman spectrometer), X-ray diffraction
(XRD), SEM (SEM), film tensile strength tester and vector network analyzer (Network
Analyzers) product is characterized.Wherein SEM can observe the sight pattern of product, and XRD can carry out Crystalline form analysis to product, thin
Film stretching strength tester can be with the suction ripple efficiency of test product with the mechanical property of test product, vector network analyzer.
Specific test data is as follows：
Fig. 1 a are Ti3C2MXene surface sweeping sem image, it can be seen that after HF is etched, originally Ti3AlC2Material
Aluminium is etched away, so as to form the layer structure of two dimension；Fig. 1 b are Ti3C2MXene/PVA scanning electron microscope image,
Ti3C2MXene and PVA forms the composite construction of stratiform.
Fig. 2 is Ti3C2MXene and Ti3C2MXene/PVA XRD picture, Ti3AlC2In Al after HF is etched significantly
Reduce, and the peak of PVA (101) is occurred in that after compound with PVA, show after compound, Ti3C2MXene/PVA composite shapes
Into.
Fig. 3 a are Ti3C2Raman image, wherein 130cm-1、430cm-1And 619cm-1, it is Ti3C2Ti-C vibration
Peak；Fig. 3 b are Ti3C2MXene/PVA Raman image, 401cm-1And 597cm-1The appearance explanation at peak is formd after adding PVA
Ti-O keys.
Fig. 4 is Ti3C2The stress strain curve of MXene/PVA composite film materials, wherein Ti3C2MXene and PVA mass ratio
For 1:1, it can be seen that the elongation at break nearly 10% of composite, intensity can reach 136MPa.
Fig. 5 is the Ti of different-thickness3C2The suction ripple effect test result of MXene/PVA composites, wherein Ti3C2MXene
Mass ratio with PVA is 1:1, composite is under thin thickness, such as 2mm thickness, and 75dB can be reached by inhaling ripple efficiency.This
It is unapproachable in like product before, as mass ratioes of the MXene in whole composite is improved, inhales ripple efficiency also
Can small elevation.Ti3C2/ PVA composites have absorption band wide, for example, 3-22GHz, inhales the characteristics of ripple efficiency is good.
The present invention is just prepared for Ti only by solution mixing3C2MXene/ polymer composites.Technique is simple, cost
Waste gas and waste liquid low and that pollution environment will not be produced；Ti prepared by the present invention3C2MXene/ polymer composites wave absorbtions
The good, absorption band of energy is wide, base material attachment is good, density is low, intensity is high, be expected to the composite wave-suction material as a new generation.
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Any modifications, equivalent substitutions and improvements made within principle etc., should be included in the scope of the protection.
Claims (5)
1. a kind of Ti3C2The preparation method of MXene/ polymer composite wave-suction materials, it is characterised in that：
S1：Ti3C2MXene preparation；
S11：Quantitatively weigh the Ti of MAX phases3AlC2, it is dissolved in the HF that concentration is 50%, it is reacted 18- under agitation
24h；
S12：Dry, that is, obtain after the reaction solution filtering in step S11 and massive laundering solid, then under 40 degree of -60 degree
Ti3C2MXene powder；
S2：Ti3C2The preparation of MXene/ thin polymer films；
S21:Quantitatively weigh Ti3C2MXene powder, and be dissolved in dimethyl sulfoxide solution, the ultrasound 15-30min under 100w-300w；
S22:By the Ti in step S213C2MXene solution and mixed with polymers, stir 1-2h；Wherein, Ti3C2MXene is with polymerizeing
The mass ratio of thing is 1：9-9：1；
S23:By Ti3C2MXene polymer solutions are in 100w ultrasounds 0.5-1h；
S24:By Ti3C2MXene polymer solutions centrifuge 15min-30min under 2000-3000rpm；And by obtained solid powder
24h is dried in end under 40-60 degree, obtains Ti3C2MXene/ polymer compound powders end；
S25:By Ti3C2MXene/ polymer compound powders end is dissolved in water and Ti is made later3C2MXene/ thin polymer films.
2. preparation method according to claim 1, it is characterised in that：In step S25：By Ti3C2MXene/ polymer is combined
Powder is dissolved in after water, then obtains Ti by filtering or spin coating3C2MXene/ thin polymer films.
3. preparation method according to claim 1, it is characterised in that：In step S22：Polymer be PVA or PMMA or
PVDF or PEI or PS.
4. preparation method according to claim 1, it is characterised in that：In step S22：Ti3C2MXene and polymer matter
Amount is than being 1：1.
5. preparation method according to claim 1, it is characterised in that：In step S11：Quantitatively weigh the Ti of MAX phases3AlC2
For in 1g, also, step S21：Quantitatively weigh Ti3C2MXene powder is 1g.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264885A (en) * | 2018-01-18 | 2018-07-10 | 北京林业大学 | A kind of electromagnetic shielding film of mechanics enhancing and preparation method thereof |
| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
| CN108441287A (en) * | 2018-04-25 | 2018-08-24 | 青岛大学 | A kind of preparation method of the nano combined er materials of Mxene/PS |
| CN109348694A (en) * | 2018-09-13 | 2019-02-15 | 上海大学 | High-strength flexible self-supporting electromagnetic wave shield film and preparation method thereof |
| CN110105087A (en) * | 2018-10-10 | 2019-08-09 | 西南交通大学 | A kind of Ti3C2The regulation method of film surface functional group |
| CN110176580A (en) * | 2019-04-25 | 2019-08-27 | 浙江大学 | A kind of Si base MAX prepares the method and application of MXenes and MXenes/P anode material |
| CN110312766A (en) * | 2018-01-25 | 2019-10-08 | 株式会社Lg化学 | Coating composition, film and electromagnetic interference shield composite material |
| CN110330646A (en) * | 2019-06-21 | 2019-10-15 | 广东工业大学 | A kind of flexible polyimide base compound dielectric film material and its preparation method and application |
| CN111270414A (en) * | 2020-03-23 | 2020-06-12 | 清华大学深圳国际研究生院 | Flexible piezoelectric fiber membrane and preparation method and application thereof |
| CN111333982A (en) * | 2020-03-13 | 2020-06-26 | 中国科学院兰州化学物理研究所 | Polytetrafluoroethylene friction material and preparation method and application thereof |
| CN111785534A (en) * | 2020-06-08 | 2020-10-16 | 华中科技大学 | Method for immobilizing MXene by ionic liquid covalent bonding and product thereof |
| CN111995831A (en) * | 2020-09-09 | 2020-11-27 | 南昌航空大学 | MXene-doped polyvinylidene fluoride composite material and preparation method thereof |
| CN112763551A (en) * | 2020-12-29 | 2021-05-07 | 电子科技大学 | Nitrogen dioxide sensor based on composite material blocking effect and preparation method thereof |
| CN112768835A (en) * | 2021-01-07 | 2021-05-07 | 陈云 | Cr (chromium)3AlC2Preparation method of/PVDF-PVA lithium ion battery diaphragm |
| CN113025271A (en) * | 2021-03-25 | 2021-06-25 | 电子科技大学 | Ti3C2TxPreparation method of MXene @ ZnO composite wave-absorbing material |
| CN113115581A (en) * | 2021-04-13 | 2021-07-13 | 郑州大学 | Ti3C2Tx composite and preparation method thereof |
| CN113773675A (en) * | 2021-09-13 | 2021-12-10 | 中国科学技术大学 | Aerogel composite thermal insulation layer and preparation method and application thereof |
| CN116178959A (en) * | 2023-02-23 | 2023-05-30 | 中国石油大学(华东) | Graphene acousto-electric signal conversion film, preparation method, detector and sensing device |
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| CN110312766A (en) * | 2018-01-25 | 2019-10-08 | 株式会社Lg化学 | Coating composition, film and electromagnetic interference shield composite material |
| CN108342036B (en) * | 2018-03-26 | 2020-05-15 | 南昌航空大学 | Magnetic Mxenes polymer composite wave-absorbing material and preparation method thereof |
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| CN111995831A (en) * | 2020-09-09 | 2020-11-27 | 南昌航空大学 | MXene-doped polyvinylidene fluoride composite material and preparation method thereof |
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