CN108620003A - The telescopic preparation method with the high MXene/ graphene composite aerogels for being electromagnetically shielded effect - Google Patents
The telescopic preparation method with the high MXene/ graphene composite aerogels for being electromagnetically shielded effect Download PDFInfo
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- CN108620003A CN108620003A CN201810514577.2A CN201810514577A CN108620003A CN 108620003 A CN108620003 A CN 108620003A CN 201810514577 A CN201810514577 A CN 201810514577A CN 108620003 A CN108620003 A CN 108620003A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses a kind of telescopic preparation methods with the high MXene/ graphene composite aerogels for being electromagnetically shielded effect, the method is compound by carrying out MXene and redox graphene, induces redox graphene and MXene and cold dry-cure means to form the three-dimensional network shape composite aerogel with abundant pore structure using modifying agent.The present invention is by uniformly being mixed redox graphene with MXene dispersion liquids, and introduce modifying agent, it finally carries out cold dry-cure and the telescopic MXene/ graphene composite aerogels with high electromagnetic shielding effect just can be obtained, reduce the bulk density of MXene, new macro morphology is constructed, and mechanical property is extremely excellent, has scalability, has pushed MXene in the application feasibility of aerospace field.
Description
Technical field
The invention belongs to nanocomposite preparing technical fields, are related to a kind of system of MXene/ graphenes composite aerogel
Preparation Method.
Background technology
MXene is a kind of two-dimentional transition metal carbide or carbonitride having similar to graphene-structured, usually
By etching or peeling off obtained by the A layer elements in MXA phases.For MAX phases, M refers to transition metal element, and A is often referred to
IIIA, IVA race element, X refer to carbon or nitrogen.
MXene possesses outstanding good electric conductivity same as graphene, be it is a kind of with metallic conduction characteristic novel two
Material is tieed up, there is extremely excellent capability of electromagnetic shielding.But general MXene materials are macroscopical in the form of powdery or film
Existing, structure extremely densification causes density larger, and structure is easily destroyed without scalability, serious influence
Applications of the MXene in electromagnetic shielding field.Because the lighter be generally intended to electromagnetic shielding material in practical applications the better,
And there is excellent mechanical property, in particular in aerospace field.In addition MXene materials are due to lamella flexibility
Not as good as graphene, it is difficult that the graphene aerogel of three-dimensional structure is constituted as being similar to graphene to be in itself, but current people
Highly desirable find a kind of method and can construct out similar to three-dimensional structure MXene as graphene.From it has been reported that cross
It is found that being the graphene aerogel for being readily formed three-dimensional appearance using redox graphene in lot of documents.And it restores
Surface of graphene oxide contains abundant oxygen-containing functional group, and there are stronger electrostatic repulsions for interlayer, to redox graphene
Aqueous dispersions be a kind of electronegative colloid, can very stable there are the several months without precipitating.It is obtained by hf etching
Also to contain hydrophilic radicals, its aqueous dispersions such as hydroxyl and epoxy group also negatively charged on the surfaces MXene.Therefore oxygen reduction fossil
Black alkene and MXene highly uniform can be dispersed with, and can be readily formed stable colloid, to light to construct out
MXene/ graphene composite aerogels provide advantageous theory support.
Invention content
It is big that there are density in order to solve common MXene materials, and structure destructible does not have scalability, limits it in electromagnetism
The problem further applied in shielding field, the present invention provides a kind of telescopic MXene/ with high electromagnetic shielding effect
The preparation method of graphene composite aerogel.The present invention is by uniformly being mixed redox graphene and MXene dispersion liquids
It closes, and introduces modifying agent, finally carry out cold dry-cure and the telescopic MXene/ with high electromagnetic shielding effect just can be obtained
Graphene composite aerogel reduces the bulk density of MXene, has constructed new macro morphology, and mechanical property is extremely excellent
It is different, there is scalability, pushed MXene in the application feasibility of aerospace field.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of the telescopic MXene/ graphene composite aerogels with high electromagnetic shielding effect, pass through by
MXene and redox graphene progress are compound, and modifying agent is utilized to induce redox graphene and MXene and cold dry-cure
Means form the three-dimensional network shape composite aerogel with abundant pore structure.Specific implementation step is as follows：
Step 1: redox graphene is scattered in deionized water, it is 4 ~ 10 to obtain redox graphene solution concentration
mg mL-1Solution A.
In this step, the redox graphene is the redox graphene of large stretch of single layer, and size is 2 ~ 5 μm.
Step 2: by a concentration of 1 ~ 3 mg mL-1MXene dispersion liquids and solution A according to mass ratio be 1 ~ 10:1 ratio
Mixing, obtains mixed solution B.
In this step, the MXene dispersion liquids are by hf etching Ti3AlC2And be prepared into.
It is ultrasonically treated again Step 3: mixed solution B first to be carried out to magnetic agitation, obtains uniformly mixed solution C.
In this step, the rotating speed of the magnetic agitation is 200 ~ 600 r/min, and the duration is 10 ~ 30 min.
In this step, the ultrasonic power is 100 ~ 300 W, and ultrasonic time is 10 ~ 30 min.
Step 4: modifying agent is added in solution C, first carries out magnetic agitation and be ultrasonically treated again, obtain solution D.
In this step, the modifying agent is dopamine, chitosan, cellulose nano-fibrous, sodium alginate and polyethylene
It is a kind of or a combination thereof in alcohol.
In this step, the dosage of the modifying agent is 3 ~ 5 wt% of solution D.
In this step, the rotating speed of the magnetic agitation is 200 ~ 600 r/min, and the duration is 10 ~ 30 min.
In this step, the ultrasonic power is 100 ~ 300 W, and ultrasonic time is 10 ~ 30 min.
Step 5: solution D is freeze-dried, MXene/ graphene composite aerogels are obtained.
In this step, the temperature of the freeze-drying is -50 ~ -80 DEG C, and the time is 48 h.
The above method prepare telescopic MXene/ graphenes composite aerogel can be applied to aerospace in terms of electricity
In magnetic screen field.
Compared with the prior art, the invention has the advantages that：
1, present invention the characteristics of easily forming three-dimensional structure using redox graphene, by redox graphene and MXene into
Row is compound, and modifying agent is added and forms three-dimensional network-like structure to can induce MXene, greatly reduces MXene material macroscopic views
The big chip architecture of the density of accumulation, MXene and redox graphene can wrap modifying agent to keep intrinsic height electricity
Conductance, and modifying agent can enhance the mechanical strength of whole composite aerogel, and its excellent scalability is assigned, finally construct
Go out a kind of three-dimensional network shape and the MXene/ graphene composite aerogels with good scalability, and creates a kind of new
MXene macroscopic views accumulate pattern, have widened its application field.
2, the present invention can further strengthen MXene and exist by introducing the graphene with excellent mechanical performance in MXene
The application potential of electromagnetic shielding field in practice.
3, the method for the present invention is extremely simple, and raw materials used at low cost, easily industrialized mass production.
4, composite aerogel prepared by the present invention compared to conventional graphene aerogel while having extremely excellent electricity
Conductance and scalability.
Description of the drawings
Fig. 1 is the telescopic MXene/ graphene composite aerogels with high electromagnetic shielding effect prepared by embodiment 1
Exemplar；
Fig. 2 is sweeping for the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect prepared by embodiment 2
Retouch electron micrograph；
Fig. 3 is the telescopic MXene/ graphene composite materials with high electromagnetic shielding effect prepared by embodiment 1-3
Electromagnet shield effect figure.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiment, however, it is not limited to this, every right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit of the technical scheme of the invention and range, should all be contained
It covers in protection scope of the present invention.
Embodiment 1：
The telescopic MXene/ graphene composite aerogel preparation methods with high electromagnetic shielding effect provided in this embodiment
Through the following steps that realize：
Step 1: redox graphene is configured to a concentration of 4 mg mL-1Redox graphene solution, ie in solution A.
Step 2: passing through hf etching Ti3AlC2MXene dispersion liquids are prepared, are used in combination the deionized water to control its concentration
For 1.5 mg mL-1.By MXene dispersion liquids and solution A according to mass ratio 1:1 ratio is mixed, and solution B is obtained.
Step 3: solution B line is carried out in the case where rotating speed is 600 r/min after magnetic agitation 30min at the ultrasound of 40 min
Reason, obtains solution C, and ultrasonic power is 200 W.
Step 4: dissolving polyvinyl alcohol in deionized water, it is added in solution C according to the ratio of 5wt%, so
Afterwards by it at 400 r/min magnetic agitation 20min, the supersound process of 10 min is then carried out under the ultrasonic power of 100W,
Obtain composite solution D.
Step 5: uniformly mixed composite solution D is freeze-dried 48h at -60 DEG C, it is compound to obtain MXene/ graphenes
Aeroge.
Fig. 1 is the telescopic MXene/ graphene composite aerogels with high electromagnetic shielding effect manufactured in the present embodiment
Exemplar.As seen from Figure 1, the MXene/ graphene composite aerogels prepared by the present embodiment have excellent compressible and stretch
Contracting performance.
Embodiment 2：
The telescopic preparation side with the high MXene/ graphene composite aerogels for being electromagnetically shielded effect provided in this embodiment
Method through the following steps that realize：
Step 1: redox graphene is configured to a concentration of 10 mg mL-1Redox graphene solution, ie in solution
A。
Step 2: passing through hf etching Ti3AlC2MXene dispersion liquids are prepared, are used in combination deionized water to be configured to a concentration of
3 mg mL-1.By MXene dispersion liquids and solution A according to mass ratio 1:2 ratio is mixed, and solution B is obtained.
Step 3: solution B is first carried out in the case where rotating speed is 300 r/min after magnetic agitation 20min at the ultrasound of 30 min
Reason obtains solution C, and ultrasonic power is 100 W.
Step 4: preparing the TRIS buffer that pH is 8.5, solution C is then added, and stir evenly,
Then by the dopamine of 4 wt% be added and the magnetic agitation 20min at 400 r/min, later under the ultrasonic power of 100W into
The supersound process of 10 min of row, obtains composite solution D.
Step 5: uniformly mixed composite solution D is freeze-dried 48h at -80 DEG C, it is compound to obtain MXene/ graphenes
Aeroge.
The telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect manufactured in the present embodiment are swept
It is as shown in Figure 2 to retouch electron micrograph.As seen from Figure 2, the compound airsetting of MXene/ graphenes prepared by the present embodiment
Glue has three-dimensional network-like structure, and pore-size is larger, reaches microns up to a hundred, therefore assigns its stretching similar to sponge
Contracting performance.
Embodiment 3：
The telescopic MXene/ graphene composite aerogel preparation methods with high electromagnetic shielding effect provided in this embodiment
Through the following steps that realize：
Step 1: redox graphene is configured to a concentration of 6 mg mL-1Redox graphene solution, ie in solution A.
Step 2: passing through hf etching Ti3AlC2MXene dispersion liquids are prepared, are used in combination the deionized water to control its concentration
For 2 mg mL-1.By MXene dispersion liquids and solution A according to mass ratio 1:3 ratio is mixed, and solution B is obtained.
Step 3: solution B is first carried out in the case where rotating speed is 500 r/min after magnetic agitation 10min at the ultrasound of 30 min
Reason obtains solution C, and ultrasonic power is 150 W.
Step 4: the cellulose nano-fibrous of 3wt% is added in solution C, then by it at 200 r/min magnetic force
150min is stirred, the supersound process of 200 min is then carried out under the ultrasonic power of 150W, obtains composite solution D.
Step 5: uniformly mixed composite solution D is freeze-dried 48h at -70 DEG C, it is compound to obtain MXene/ graphenes
Aeroge.
The telescopic electricity with the high MXene/ graphene composite materials for being electromagnetically shielded effect prepared by embodiment 1-3
Magnetic screen efficiency figure is as shown in Figure 3.From the figure 3, it may be seen that increasing with MXene additive amounts, the electromagnetic screen of gained composite aerogel
Cover efficiency enhancing.1 gained composite aerogel electromagnet shield effect of embodiment up to 20 ~ 25 dB, far above in practical application for
The minimum requirements of electromagnet shield effect.3 gained composite aerogel electromagnet shield effect of embodiment is up to 30 ~ 50 dB, therefore is navigating
Electromagnetic shielding application field in terms of empty space flight has great potentiality.
Claims (9)
1. a kind of telescopic preparation method with the high MXene/ graphene composite aerogels for being electromagnetically shielded effect, feature
Being the method, steps are as follows：
Step 1: redox graphene is scattered in deionized water, it is 4 ~ 10 to obtain redox graphene solution concentration
mg mL-1Solution A；
Step 2: by a concentration of 1 ~ 3 mg mL-1MXene dispersion liquids and solution A according to mass ratio be 1 ~ 10:1 ratio is mixed
It closes, obtains mixed solution B；
It is ultrasonically treated again Step 3: mixed solution B first to be carried out to magnetic agitation, obtains uniformly mixed solution C；
Step 4: modifying agent is added in solution C, first carries out magnetic agitation and be ultrasonically treated again, obtain solution D；
Step 5: solution D is freeze-dried, MXene/ graphene composite aerogels are obtained.
2. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the redox graphene is the redox graphene of large stretch of single layer, and size is 2 ~ 5 μm.
3. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the MXene dispersion liquids are by hf etching Ti3AlC2And be prepared into.
4. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the rotating speed of the magnetic agitation is 200 ~ 600 r/min, and the duration is 10 ~ 30 min.
5. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the ultrasonic power is 100 ~ 300 W, and ultrasonic time is 10 ~ 30 min.
6. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the modifying agent is dopamine, chitosan, cellulose nano-fibrous, sodium alginate and poly- second
It is a kind of or a combination thereof in enol.
7. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the dosage of the modifying agent is 3 ~ 5 wt% of solution D.
8. the telescopic MXene/ graphene composite aerogels that there is height to be electromagnetically shielded effect according to claim 1
Preparation method, it is characterised in that the temperature of the freeze-drying is -50 ~ -80 DEG C, and the time is 48 h.
9. the telescopic MXene/ with high electromagnetic shielding effect prepared by claim 1-8 any claim the methods
Graphene composite aerogel is applied in the electromagnetic shielding field in terms of aerospace.
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| CN109712824A (en) * | 2019-02-12 | 2019-05-03 | 西南交通大学 | A kind of method and three-dimensional MXene array using liquid-crystalization MXene building three-dimensional MXene array |
| CN109851313A (en) * | 2019-01-22 | 2019-06-07 | 华南理工大学 | A kind of highly sensitive, the wide line sensing scope compressible compound carbon aerogels and its preparation and application |
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| CN110429242A (en) * | 2019-07-12 | 2019-11-08 | 大连理工大学 | A kind of compound lithium an- ode and its synthetic method based on MXene aeroge |
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| CN113645820A (en) * | 2021-07-12 | 2021-11-12 | 西安理工大学 | Preparation method of MXene-CNT/carbon aerogel composite material |
| CN113645820B (en) * | 2021-07-12 | 2023-12-26 | 西安理工大学 | Preparation method of MXene-CNT/carbon aerogel composite material |
| CN113979430A (en) * | 2021-10-21 | 2022-01-28 | 中国科学院兰州化学物理研究所 | GO/MXene composite aerogel, preparation method thereof and multi-environment sensing application |
| CN114905803B (en) * | 2022-04-08 | 2023-11-24 | 中国科学院宁波材料技术与工程研究所 | Composite material with heat conduction and electromagnetic protection functions and preparation method and application thereof |
| CN114905803A (en) * | 2022-04-08 | 2022-08-16 | 中国科学院宁波材料技术与工程研究所 | Composite material with heat conduction and electromagnetic protection functions and preparation method and application thereof |
| CN115094621A (en) * | 2022-07-04 | 2022-09-23 | 安徽工程大学 | Skin-core type MXene fiber aerogel and preparation method thereof |
| CN115746392A (en) * | 2022-11-25 | 2023-03-07 | 中国科学院海洋研究所 | Modified friction power generation sponge, single-electrode sponge friction power generation device, and preparation and application thereof |
| CN115746392B (en) * | 2022-11-25 | 2023-12-19 | 中国科学院海洋研究所 | Modified friction power generation sponge, single-electrode sponge friction power generation device, and preparation and application thereof |
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