CN109152318A - A kind of preparation method of novel electromagnetic wave absorbent material - Google Patents
A kind of preparation method of novel electromagnetic wave absorbent material Download PDFInfo
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Abstract
The invention belongs to the fields of the preparation of nano material and electromagnetic wave absorbent material, are related to a kind of preparation method of novel electromagnetic wave absorbent material, with ethyl alcohol or deionized water and Nb2AlC MAX is raw material, synthesizes Nb using HF (hafnium) etching and hydro-thermal method2C MXene nanometer sheet and while adjust its interlamellar spacing and surface group, and any surfactant or template need not be added, it need to first use Nb2AlC precursor prepares pure Nb2C MXene, then the pure Nb to preparation2C MXene is improved by way of hydro-thermal and improved Nb is made2C MXene nanometer sheet;Nb2C MXene nanometer sheet has good electromagnetic wave absorption performance, while absorption band range is wide, can be used as absorbing material, can be applied to electromangnetic spectrum field and fight stealth technology field, and technical process is environmentally protective;Simple to be convenient for operation, raw material is easy to get, and preparation cost is low;Preparation efficiency is high, and good product quality obtained, stability is strong, can be realized large-scale production manufacture, application environment is good, wide market.
Description
Technical field:
The invention belongs to the fields of the preparation of nano material and electromagnetic wave absorbent material, are related to a kind of novel electromagnetic wave suction
The preparation method of material is received, with ethyl alcohol or deionized water and Nb2AlC MAX is raw material, is closed using HF (hafnium) etching and hydro-thermal method
At Nb2C MXene nanometer sheet and while adjust its interlamellar spacing and surface group, and need not be added any surfactant or
Template.
Background technique:
The electromagnetic wave absorbent material of efficient lightweight seriously affects people to overcoming Contamination of Electromagnetic Wave to play a crucial role
Body health, reduces the performance of electronic equipment.In recent years, various new E MW absorbers have been developed that anti-electromagnetic wave
Radiation and interference.Wherein, two-dimensional structure material such as graphene and transition metal oxide (or sulfide) due to its special two
Tie up structure, high aspect ratio, high surface area, low-density, thickness of thin layer and good mechanical strength.Unfortunately, to being at present
Only, pure two-dimensional material shows low absorption performance due to its limited loss mode.For example, it was reported that the oxygen of electronation
Graphite alkene shows poor electromaganic wave absorbing property, and due to a thickness of minimal reflection loss when 2.0mm be only about-
7.0dB shows that pure graphene is difficult to meet the practical application of electro-magnetic wave absorption.And for molybdenum disulfide, most representative base
Show that minimum RL value is -38.2dB in the EMW absorbing material of two-dimentional transient metal sulfide, with a thickness of 2.4mm.Although with pure stone
Black alkene is compared, and this absorbability significantly improves, but still has more spaces to develop based on the more efficient of two-dimensional material
Electromagnetism wave material.
MXene(Mn+1XnTx) it is a kind of two dimension layering early stage transition metal carbide, nitride or carbonitride, exist recently
Various research fields such as supercapacitor, electro-catalysis, bionic enzyme etc. attract extensive attention.Their molecular formula is Mn+1XnTx,
Middle M represents early stage transition metal (such as titanium, niobium and molybdenum etc.), and X represents carbon or nitrogen, n=1,2 or 3, TxCorresponding to some water-wetted surfaces
End-capping group, such as-OH ,-O and-F.It is different from traditional 2D material, MXene material due to its surface functional group presence and draw
Significant inherent shortcoming is played, this may cause increased depolarising and reduced conductivity.Therefore, their prototypical member
Ti3C2TxMXene also starts to show infusive electro-magnetic wave absorption ability, this shows huge MXene family in electromagnetism
Wave absorbs field and absorbs with huge application potential.However, in order to prepare efficiently based on Ti3C2TxThe electromagnetic wave of MXene
Absorbing material, it generally has to form hybrid by the technique of some energy-intensives and complexity to increase its dielectric loss.
For example, obtaining Ti by catalytic chemical vapor deposition technique3C2TxMXene and carbon nano-tube hybridization material pass through short annealing work
Skill adjusts Ti3C2TxThe surface texture of MXene forms carbon/titanium dioxide hybrid material by the carbon-coating that high temperature removes MXene
Deng.Previous studies show the pure Ti after n,N-Dimethylformamide solvent heat treatment3C2TxMXene may be used as base
In the electromagnetic wave absorbent material of dielectric loss, this is because increasing interlamellar spacing, but environmental problem (N, N- diformazan is still had
Base formamide has carcinogenicity).Therefore, design prepares a kind of preparation method of novel electromagnetic wave absorbent material, can be with simpler
Single and environmental protection mode develops novel MXene type electromagnetic wave absorption material, to obtain superior absorbent properties.
Summary of the invention:
It is an object of the invention to overcome disadvantage present on the prior art, design a kind of green, succinct, effective novel
Electromagnetic wave absorbent material preparation method, preparation efficiency is high, good product quality obtained.
To achieve the goals above, the preparation method of the novel electromagnetic wave absorbent material of one kind of the present invention passes through system
Standby Nb2CTxMXene nanometer sheet simultaneously passes through hydro-thermal method to the further improved technique of its electromagnetic wave absorption performance, concrete technology step
Suddenly it is carried out as follows:
S1, Nb is used2AlC precursor prepares pure Nb2C MXene;
(1), 4g Nb is weighed2AlC powder is put into 250mL polypropylene vial, and is put on magnetic stirring apparatus, and revolving speed is greater than
200 revs/min;
(2), 1g Nb is pressed in the polypropylene vial in step (1)2The ratio of AlC:20mL hydrofluoric acid solution is slowly added dropwise
The hydrofluoric acid solution that 80mL mass fraction is 49% reacts 150h or more under the stirring greater than 200 rpms at room temperature;
(3), it is put into centrifuge tube after after reaction taking out the suspension in polypropylene vial, centrifuge tube is symmetrically placed
In in centrifuge, with revolving speed centrifugation 10 minutes or more greater than 7000 revs/min, solution after centrifugation is made, is excessive hydrogen fluorine
Acid, impurity containing aluminium and Nb2C MXene, its lower sediment is pure Nb after centrifugation2C MXene;
(4), by pure Nb2C MXene washs centrifugation with deionized water repeatedly, until its neutrality, to remove extra fluorine
Ion and hydrogen ion;
(5), by pure Nb obtained in step (4)2C MXene solid be greater than 50 DEG C at be dried in vacuo 8 hours or more it is standby
With;
S2, to the pure Nb prepared in step S12C MXene is improved by way of hydro-thermal:
(1), the pure Nb of 0.25g is weighed respectively in two clean beakers2C MXene powder, it is one of that 20mL is added
Deionized water, another is added 20mL dehydrated alcohol, it is spare to obtain black suspension after stirring;
(2), black suspension prepared by step (1) is transferred in closed PTFE vessel and is put into hydrothermal reaction kettle
In, 100 DEG C at a temperature of hydro-thermal 10 hours, be made hydro-thermal after suspension;
(3), after the suspension natural conditions after hydro-thermal drop to room temperature, the polytetrafluoroethylene (PTFE) in hydrothermal reaction kettle is taken out
Tank, and will liquid in polytetrafluoroethyltank tank take out after be put into centrifuge tube, centrifuge tube is symmetrically placed in centrifuge, with big
Be centrifuged 10 minutes in 10000 revs/min of revolving speeds or more, upper layer is colorless and transparent solvent after centrifugation, and lower layer is improved
Nb2C MXene nanometer sheet;
(4), it takes lower sediment in step (3) to wash centrifugation 2-3 times repeatedly, and is dried in vacuo 8 hours in the case where being greater than 50 DEG C
The improved multilayer Nb obtained above2C MXene nanometer sheet.
Pure Nb of the present invention to preparation2C MXene and improved stratiform Nb2The electromagnetic wave absorbability of C MXene nanometer sheet
It can be carried out test, find improved stratiform Nb2The electromagnetic wave absorption performance of C MXene nanometer sheet has larger improvement, especially
Solvent is made with ethyl alcohol and obtains nanometer sheet when absorbed layer is with a thickness of 2.9 millimeters, and optimal absorbing property is obtained at 3.93GHz,
Highest reflection loss reaches -52.2dB, and absorption efficiency can achieve 99.999%, and absorption band is wider, in 2.0-4.0GHz
There is higher electro-magnetic wave absorption;And the electro-magnetic wave absorption intensity of the nanometer sheet obtained with water as solvent is slightly less than and uses ethanol as solvent
Obtained nanometer sheet, but absorption band range is wider;Show improved stratiform Nb2C MXene nanometer sheet is extraordinary suction
Wave material can be applied to electromangnetic spectrum field and fight stealth technology field and add to improve the compatibility of electromagnetic equipment
By force to the protection of information technology, the preferably health of the personnel of protection operation electromagnetic radiation equipment.
Compared with prior art, the present invention using ethyl alcohol or deionized water as solvent in preparation process, without using
Surfactant designs a kind of preparation method of new electromagnetic wave absorbent material as template, and technical process is environmentally protective;Letter
Single to be convenient for operation, raw material is easy to get, and preparation cost is low;Preparation efficiency is high, and good product quality obtained, stability is strong, Neng Goushi
Existing large-scale production manufacture, application environment is good, wide market.
Detailed description of the invention:
Fig. 1 is stratiform Nb of the present invention2The preparation principle schematic diagram of C MXene nanometer sheet.
Fig. 2 is improved stratiform Nb of the present invention2The electro-magnetic wave absorption mechanism schematic diagram of C MXene nanometer sheet.
Fig. 3 A and Fig. 3 B are the scanning electron microscopic picture that dehydrated alcohol of the present invention makees nanometer sheet after Solvents Solvent heat;
Fig. 3 C and Fig. 3 D are the scanning electron microscopic picture that deionized water of the present invention makees nanometer sheet after solvent hydro-thermal.
Fig. 4 A is the electromagnetic wave absorption performance test knot of the present invention for spending nanometer sheet after ethanol as solvent solvent heat
Fruit figure;Fig. 4 B is the electromagnetic wave absorption performance test result that deionized water of the present invention makees nanometer sheet after solvent hydro-thermal
Figure.
Specific embodiment:
Below by example with reference, the present invention is further described.
Embodiment 1:
The preparation method of the novel electromagnetic wave absorbent material of one kind that the present embodiment is related to, the specific process step of this method
It is carried out as follows:
S1, Nb is used2AlC precursor prepares pure Nb2C MXene;
(1), 4g Nb is weighed2AlC powder is put into 250mL polypropylene vial, and is put on magnetic stirring apparatus, and revolving speed is arranged
300 revs/min;
(2), toward pressing 1g Nb in the polypropylene vial of step (1)280mL is slowly added dropwise in the ratio of AlC:20mL hydrofluoric acid solution
The hydrofluoric acid solution that mass fraction is 49%, reacts 180h under 300 rpms of stirring at room temperature, after hydro-thermal is made
Suspension is spare;
(3), it is put into centrifuge tube after after reaction taking out the suspension in polypropylene vial, centrifuge tube is symmetrically placed
In in centrifuge, with revolving speed centrifugation 15 minutes or more of 9000 revs/min, solution after centrifugation is made, lower sediment is pure
Nb2C MXene and some aluminum contained compound impurity;
(4), by step (3) pure Nb2Centrifugation 15 times is washed with deionized in C MXene, until its pH value is about 7, to remove
Remove extra fluorine ion and hydrogen ion;
(5), by pure Nb made from step (4)2C MXene solid be dried in vacuo at 60 DEG C 10 hours it is spare;
S2, to the pure Nb prepared in step S12C MXene is improved by way of hydro-thermal:
(1), the pure Nb of 0.25g is weighed respectively in two clean beakers2C MXene powder, it is one of that 20mL is added
Deionized water, another is added 20mL dehydrated alcohol, it is spare to obtain black suspension after mixing evenly;
(2), solution prepared by step (1) is transferred in closed PTFE vessel and is put into hydrothermal reaction kettle,
Hydro-thermal 10 hours at a temperature of 100 DEG C, the suspension after hydro-thermal is made are solvent, some oxide impurities and improved multilayer
Nb2C MXene nanometer sheet;
(3), after the solution natural conditions after hydro-thermal drop to room temperature, the polytetrafluoroethylene (PTFE) in hydrothermal reaction kettle is taken out
Tank, and will liquid in polytetrafluoroethyltank tank take out after be put into centrifuge tube, centrifuge tube is symmetrically placed in centrifuge, with
Revolving speed centrifugation 15 minutes or more of 12000 revs/min, upper layer is colorless and transparent solvent after centrifugation, and lower layer is improved
Nb2C MXene nanometer sheet and some foreign ions;
(4) it takes in step (3) lower sediment washing centrifugation 3 times, and is dried in vacuo changing of obtaining for 10 hours at 60 DEG C
Multilayer Nb after2C MXene nanometer sheet;
Embodiment 2:
The present embodiment 2 is to the Nb prepared in embodiment 12The electromagnetic wave absorption performance of C MXene nanometer sheet is tested, and is surveyed
Test result is as shown in Figure 4, it has been found that improved stratiform Nb2The electromagnetic wave absorption performance of C MXene nanometer sheet has larger change
It is kind, solvent especially is made with ethyl alcohol and obtains nanometer sheet when absorbed layer is with a thickness of 2.9 millimeters, is obtained at 3.93GHz optimal
Absorbing property, highest reflection loss reach -52.2dB, and absorption efficiency can achieve 99.999%, and absorption band is wider,
2.0-4.0GHz there is higher electro-magnetic wave absorption;And the electro-magnetic wave absorption intensity of the nanometer sheet obtained with water as solvent is slightly less than use
The nanometer sheet that ethanol as solvent obtains, but absorption band range is wider;Show the stratiform Nb prepared in embodiment 12C MXene receives
Rice piece is extraordinary absorbing material, can be applied to electromangnetic spectrum field and fight stealth technology field, can be improved
The compatibility of electromagnetic equipment reinforces the protection to information technology, the preferably body of the personnel of protection operation electromagnetic radiation equipment
Health.
Claims (5)
1. a kind of preparation method of novel electromagnetic wave absorbent material, it is characterised in that specific process step as follows into
Row:
S1, Nb is used2AlC precursor prepares pure Nb2C MXene;
(1), 4g Nb is weighed2AlC powder is put into 250mL polypropylene vial, and is put on magnetic stirring apparatus, revolving speed be greater than 200 turns/
Minute;
(2), 1g Nb is pressed in the polypropylene vial in step (1)280mL matter is slowly added dropwise in the ratio of AlC:20mL hydrofluoric acid solution
The hydrofluoric acid solution that score is 49% is measured, reacts 150h or more at room temperature under the stirring greater than 200 rpms;
(3), after reaction will suspension in polypropylene vial take out after be put into centrifuge tube, by centrifuge tube it is symmetrically placed in from
In scheming, be centrifuged 10 minutes with the revolving speed greater than 7000 revs/min or more, solution after centrifugation is made, for excessive hydrofluoric acid, contains
Aluminium impurity and Nb2C MXene, its lower sediment is pure Nb after centrifugation2C MXene;
(4), by pure Nb2C MXene washs centrifugation with deionized water repeatedly, until its neutrality, with remove extra fluorine ion and
Hydrogen ion;
(5), by pure Nb obtained in step (4)2C MXene solid be greater than 50 DEG C at be dried in vacuo 8 hours or more it is spare;
S2, to the pure Nb prepared in step S12C MXene is improved by way of hydro-thermal:
(1), the pure Nb of 0.25g is weighed respectively in two clean beakers2C MXene powder, it is one of that 20mL deionization is added
Water, another is added 20mL dehydrated alcohol, it is spare to obtain black suspension after stirring;
(2), black suspension prepared by step (1) is transferred in closed PTFE vessel and is put into hydrothermal reaction kettle,
100 DEG C at a temperature of hydro-thermal 10 hours, be made hydro-thermal after suspension;
(3), after the suspension natural conditions after hydro-thermal drop to room temperature, the polytetrafluoroethyltank tank in hydrothermal reaction kettle is taken out,
And will liquid in polytetrafluoroethyltank tank take out after be put into centrifuge tube, centrifuge tube is symmetrically placed in centrifuge, to be greater than
Revolving speed centrifugation 10 minutes or more of 10000 revs/min, upper layer is colorless and transparent solvent after centrifugation, and lower layer is improved
Nb2C MXene nanometer sheet;
(4), it takes lower sediment in step (3) to wash centrifugation 2-3 times repeatedly, and is dried in vacuo 8 hours or more in the case where being greater than 50 DEG C
The improved multilayer Nb obtained2C MXene nanometer sheet.
2. the preparation method of the novel electromagnetic wave absorbent material of one kind according to claim 1, it is characterised in that preparation
Pure Nb2C MXene and improved stratiform Nb2C MXene nanometer sheet has good electromagnetic wave absorption performance.
3. according to claim 1 in -2 the novel electromagnetic wave absorbent material of one kind described in any claim preparation method,
It is characterized in that being the stratiform Nb that solvent obtains with ethyl alcohol2C MXene nanometer sheet when absorbed layer is with a thickness of 2.9 millimeters,
Obtaining optimal absorbing property at 3.93GHz, highest reflection loss reaches -52.2dB, and absorption efficiency can achieve 99.999%, and
Absorption band is wider, has higher electro-magnetic wave absorption in 2.0-4.0GHz.
4. according to claim 1 in -2 the novel electromagnetic wave absorbent material of one kind described in any claim preparation method,
It is characterized in that the stratiform Nb obtained with water as solvent2C MXene nanometer sheet has good electromagnetic wave absorption performance, absorbs simultaneously
Frequency range is wide.
5. according to claim 1 in -2 the novel electromagnetic wave absorbent material of one kind described in any claim preparation method,
It is characterized in that the stratiform Nb of preparation2C MXene nanometer sheet can be used as absorbing material, can be applied to electromangnetic spectrum
Field and fight stealth technology field, to reinforce the protection to information technology, are preferably protected to improve the compatibility of electromagnetic equipment
The health of the personnel of shield operation electromagnetic radiation equipment.
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CN109694074A (en) * | 2019-03-04 | 2019-04-30 | 青岛大学 | A kind of method that electrochemical process prepares MXenes and its derivates nanometer piece |
CN109911897A (en) * | 2019-03-01 | 2019-06-21 | 哈尔滨师范大学 | One-step synthesis method lacks layer Nb2The method and its application of C-material |
CN111574958A (en) * | 2020-05-19 | 2020-08-25 | 东华大学 | Carbide MXene/SiO of core-edge structure2Nano-plate-shaped ultrathin microwave absorbing material |
CN112028728A (en) * | 2020-09-11 | 2020-12-04 | 陕西科技大学 | Method for preparing cyclohexanol and cyclohexane by catalytic hydrogenation of diphenyl ether |
CN112047341A (en) * | 2020-08-31 | 2020-12-08 | 山东大学 | Nb-shaped alloy2C MXene material and preparation method and application thereof |
CN114423269A (en) * | 2022-01-24 | 2022-04-29 | 同济大学 | Nitrogen-doped MXene @ HCF electromagnetic composite wave-absorbing material and preparation method thereof |
WO2023077620A1 (en) * | 2021-11-02 | 2023-05-11 | 中国科学院深圳先进技术研究院 | Electromagnetic wave absorption material prepared on basis of mxene waste precipitate, preparation method therefor, and use thereof |
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CN109911897A (en) * | 2019-03-01 | 2019-06-21 | 哈尔滨师范大学 | One-step synthesis method lacks layer Nb2The method and its application of C-material |
CN109694074A (en) * | 2019-03-04 | 2019-04-30 | 青岛大学 | A kind of method that electrochemical process prepares MXenes and its derivates nanometer piece |
CN111574958A (en) * | 2020-05-19 | 2020-08-25 | 东华大学 | Carbide MXene/SiO of core-edge structure2Nano-plate-shaped ultrathin microwave absorbing material |
CN111574958B (en) * | 2020-05-19 | 2023-03-21 | 东华大学 | Carbide MXene/SiO of core-edge structure 2 Nano-plate-shaped ultrathin microwave absorbing material |
CN112047341A (en) * | 2020-08-31 | 2020-12-08 | 山东大学 | Nb-shaped alloy2C MXene material and preparation method and application thereof |
CN112028728A (en) * | 2020-09-11 | 2020-12-04 | 陕西科技大学 | Method for preparing cyclohexanol and cyclohexane by catalytic hydrogenation of diphenyl ether |
CN112028728B (en) * | 2020-09-11 | 2022-11-01 | 陕西科技大学 | Method for preparing cyclohexanol and cyclohexane by catalytic hydrogenation of diphenyl ether |
WO2023077620A1 (en) * | 2021-11-02 | 2023-05-11 | 中国科学院深圳先进技术研究院 | Electromagnetic wave absorption material prepared on basis of mxene waste precipitate, preparation method therefor, and use thereof |
CN114423269A (en) * | 2022-01-24 | 2022-04-29 | 同济大学 | Nitrogen-doped MXene @ HCF electromagnetic composite wave-absorbing material and preparation method thereof |
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