CN108342036A - A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof - Google Patents
A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof Download PDFInfo
- Publication number
- CN108342036A CN108342036A CN201810249523.8A CN201810249523A CN108342036A CN 108342036 A CN108342036 A CN 108342036A CN 201810249523 A CN201810249523 A CN 201810249523A CN 108342036 A CN108342036 A CN 108342036A
- Authority
- CN
- China
- Prior art keywords
- mxenes
- prepared
- composite wave
- iron oxide
- magnetism
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
A kind of preparation method of magnetism Mxenes polymer composite wave-suction materials provided by the invention, includes the following steps：Iron oxide and cetyl trimethylammonium bromide are added in deionized water, and the iron oxide dispersion liquid of cetyl trimethylammonium bromide modification is prepared in ultrasound；Mxenes (Ti are added dropwise in iron oxide dispersion liquid3C2Tx) in colloid, Mxenes (Ti are prepared in magnetic agitation3C2Tx)/ Fe2O3Suspension, then filter, dry after heating reaction, then cooled to room temperature are first carried out in argon atmosphere, Mxenes (Ti are prepared3C2Tx)/Fe3O4Nanocomposite；Kynoar and N are added, N dimethylformamides carry out ultrasound, make Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and Kynoar after mixing, are packed into mold and first carry out hot pressing, then pressurize cooling, Mxenes (Ti are prepared3C2Tx)/Fe3O4The Kynoar composite wave-suction material of filling.In the composite material that preparation method provided by the invention is prepared polymeric substrates content it is high, easily film forming, easy processing, light weight, be easy to industrialized production.
Description
Technical field
The present invention relates to field of composite material preparation more particularly to a kind of magnetism Mxenes polymer composite wave-suction material and
Preparation method.
Background technology
As Fourth Generation Fighters（American Standard, the 5th generation of Russian standard）, 20 such as F22, are destroyed, in the 4S performance indicators emphasized
Protrusion one, low detectivity（It is commonly called as " stealthy "）It is the popular domain of current Technological research, and low detectivity is in addition to leaning on
The aerodynamic configuration of aircraft itself, main is one layer of absorbing material being coated with by aircraft surfaces.And as modern radar detects
Technology is constantly progressive, and to absorbing material, more stringent requirements are proposed." thickness is thin, light weight, frequency range is wide, absorption is strong " is at working as
For the latest requirement of absorbing material, but traditional absorbing material there is density it is big, thickness is thick and frequency range is narrow the shortcomings of, it is difficult to
Meet requirement of the present age to absorbing material.
Two-dimentional transition metal carboritride（MXenes）Be just find and synthesize recent years be with MAX phase ceramics before
The two-dimensional material synthesized after body selective etch element A is driven, MXenes has typical class grapheme material, has surface function
The advantages that group is abundant, electric conductivity is strong, easy film forming.MXenes can convert the energy of electromagnetic wave to thermal energy, in absorbing material field
Have broad application prospects, MXenes is the general name of a kind of material, wherein Ti3C2Tx is studied widest a kind of.
Ti3C2The composite material of Tx and sodium alginate has embodied excellent capability of electromagnetic shielding work and has been published in 2016
On Science, but MXenes piece interlayers are easily reunited, and which has limited its performances.
Invention content
In order to solve the above technical problems, first aspect present invention provides a kind of magnetism Mxenes polymer composite wave-absorbing materials
The preparation method of material, includes the following steps：
S1：Powdered iron oxide and cetyl trimethylammonium bromide are added in deionized water, and ultrasound makes iron oxide exist
It is uniformly dispersed in deionized water, the iron oxide dispersion liquid of cetyl trimethylammonium bromide modification is prepared；
S2：Mxenes (Ti are added dropwise in the iron oxide dispersion liquid that step S1 is prepared3C2Tx) in colloid, magnetic agitation system
It is standby to obtain Mxenes (Ti3C2Tx)/ Fe2O3Suspension, then filtered with inorganic filter membrane, dried, finally obtain Mxenes
(Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3It is deposited in argon atmosphere and first carries out heating reaction,
Mxenes (Ti are prepared in cooled to room temperature again3C2Tx)/Fe3O4Nanocomposite；
S4：In the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4The mixture of nanocomposite and Kynoar
In, n,N-Dimethylformamide is added, carries out ultrasound, makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride
Alkene is uniformly mixed；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold and first carry out hot pressing, then pressurize cooling, Mxenes (Ti are prepared3C2Tx)/Fe3O4The Kynoar of filling is compound
Absorbing material.
Wherein, the iron oxide is α-Fe2O3, the α-Fe2O3It is prepared by the following method to obtain：In 100mL deionizations
2.73g Iron(III) chloride hexahydrates and 2g urea, the heating water bath 5h at 90 DEG C, while magnetic agitation are added in water, the reaction was complete
The precipitation that reaction generates is collected by centrifugation afterwards, and spends ion-cleaning, then dry 12h under the conditions of temperature is 60 DEG C, is prepared
Affiliated FeOOH is finally heated to 450 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 2h, then naturally cold by FeOOH
But to room temperature, α-Fe are prepared2O3。
Wherein, the mass ratio of the iron oxide and the cetyl trimethylammonium bromide is 1:10~1:30.
Preferably, the mass ratio of the iron oxide and the cetyl trimethylammonium bromide is 1:15,1:20,1:25.
Wherein, the solid-to-liquid ratio of the iron oxide and the deionized water is 10:100~200mg/mL.
Preferably, the solid-to-liquid ratio of the iron oxide and the deionized water is 10:120mg/mL, 10:140mg/mL, 10:
160mg/mL, 10:180mg/mL.
Wherein, the iron oxide and the Mxenes (Ti3C2Tx mass ratio) is 15:85~85:85.
Preferably, the iron oxide and the Mxenes (Ti3C2Tx mass ratio) is 20:85,30:85,40:85,50:
85,60:85,70:85,80:85.
Wherein, the Mxenes (Ti3C2Tx)/Fe3O4The mass percent of composite material and the Kynoar be 5 ~
20%:80~95%。
Preferably, the Mxenes (Ti3C2Tx)/Fe3O4The mass percent of composite material and the Kynoar is
6%:94%, 7%:93%, 8%:92%, 9%:91%, 10%:90%, 11%:89%, 12%:88%, 13%:87%, 14%:86%, 15%:85%,
16%:84%, 17%:83%, 18%:82%, 19%:81%.
Wherein, in the step S3, the condition for heating reaction is to be heated to 350 ~ 500 with the heating rate of 3 ~ 7 DEG C/min
DEG C, keep the temperature 15 ~ 45min.
Preferably, the condition for heating reaction is, 400 ~ 450 DEG C are heated to the heating rate of 4 ~ 5 DEG C/min, heat preservation 20 ~
35min。
Wherein, in the step S4, the temperature of hot pressing is 200 ~ 240 DEG C, and pressure is 10 ~ 20MPa, and the time is 2 ~ 6h.
Preferably, the temperature of hot pressing is 210 ~ 230 DEG C, and pressure is 12 ~ 18MPa, and the time is 2.5 ~ 4.5h.
Second aspect of the present invention provides a kind of magnetism Mxenes polymer composite wave-suction materials, in the composite wave-suction material
Mxenes(Ti3C2Tx)/Fe3O4The mass percent of nanocomposite is 5% ~ 20%, the Mxenes (Ti3C2Tx)/Fe3O4
Fe in nanocomposite3O4Mass percent be 14.6% ~ 49.8%, the Mxenes (Ti3C2Tx) it is four layers below few
Layer or single layer, the Fe3O4For polyhedron, grain size is 200 ~ 300nm.
Beneficial effects of the present invention：
A kind of preparation method of magnetism Mxenes polymer composite wave-suction materials provided by the invention, by simple wet-chemical and
Heat treatment is prepared, and has the following advantages：
（1）By the Mxenes (Ti of high conductivity3C2Tx) with magnetic Fe3O4It is compound to inhibit Mxenes (Ti3C2Tx) lamella
Accumulation；
（2）Using surfactant cetyl trimethylammonium bromide by α-Fe2O3Nano-particle uniformly dispersion and with
Mxenes(Ti3C2Tx) lamella uniformly contacts；
（3）It is cracked to form C at high temperature by α-Fe using the cetyl trimethylammonium bromide of remaining2O3It is reduced to Fe3O4。
（4）In the composite material polymeric substrates content it is high, easily film forming, easy processing, light weight, be easy to industrialized production.
Description of the drawings
It, below will be to needing attached drawing to be used to make letter in embodiment in order to illustrate more clearly of technical scheme of the present invention
Singly introduce, it should be apparent that, the accompanying drawings in the following description is only some embodiments of the present invention, corresponds to the general of this field
For logical technical staff, without creative efforts, other drawings may also be obtained based on these drawings；
Fig. 1 is the α-Fe that the embodiment of the present invention is prepared2O3SEM figure；
Fig. 2 is the Mxenes (Ti that the embodiment of the present invention 1 is prepared3C2Tx)/Fe3O4The SEM of nanocomposite schemes.
Specific implementation mode
It is the preferred embodiment of the present invention below, it is noted that for those skilled in the art,
Various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as this hair
Bright protection domain.
Embodiment 1
The present invention provides a kind of preparation methods of magnetism Mxenes polymer composite wave-suction materials, include the following steps：
S1：20mg powdered iron oxide and 200mg cetyl trimethylammonium bromides are added in 200mL deionized waters, and
Ultrasound makes iron oxide be uniformly dispersed in deionized water, and the iron oxide dispersion of cetyl trimethylammonium bromide modification is prepared
Liquid；
S2：The iron oxide dispersion liquid that step S1 is prepared is added dropwise to the Mxenes of a concentration of 0.1mg/mL of 800mL
(Ti3C2Tx) in colloid, for 24 hours, Mxenes (Ti are prepared in magnetic agitation3C2Tx)/ Fe2O3Suspension, then with aperture be 0.22
μm inorganic filter membrane to the Mxenes (Ti that are prepared3C2Tx)/ Fe2O3Suspension is filtered and is done under temperature 60 C
Dry 12h finally obtains Mxenes (Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3Precipitation is placed in tube furnace, in argon atmosphere, with
The heating rate of 5 DEG C/min is heated to 400 DEG C and keeps the temperature 30min, then cooled to room temperature, and black powder is prepared
Mxenes(Ti3C2Tx)/Fe3O4Nanocomposite；
S4：Weigh the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4Nanocomposite 0.05g and Kynoar
0.95g, is added solvent n,N-Dimethylformamide, and ultrasonic 1h makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and poly-
Vinylidene is uniformly mixed, then naturally dry；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold to be placed on hot press, be 200 DEG C in temperature, pressure is to be molded 4h under 10MPa, then pressurize cools down, and is prepared
Mxenes(Ti3C2Tx)/Fe3O4The Kynoar composite wave-suction material of filling.
The iron oxide is α-Fe2O3, it is prepared by the following method to obtain：
Addition 2.73g Iron(III) chloride hexahydrates and 2g urea in 100mL deionized waters, the heating water bath 5h at 90 DEG C, simultaneously
Magnetic agitation is collected by centrifugation the precipitation that reaction generates, and spends ion-cleaning after the reaction was complete, then under the conditions of temperature is 60 DEG C
Dry 12h, is prepared FeOOH, affiliated FeOOH is finally heated to 450 with the heating rate of 5 DEG C/min
DEG C, 2h, then cooled to room temperature are kept the temperature, α-Fe are prepared2O3。
The magnetic Mxenes polymer composite wave-suction material being prepared through this embodiment, in the composite wave-suction material
Mxenes(Ti3C2Tx)/Fe3O4The mass percent of nanocomposite is 5%, Mxenes in the composite wave-suction material
(Ti3C2Tx) it is four layers of few layer or single layer below, Fe3O4For polyhedron, grain size is 200 ~ 300nm.
Embodiment 1 is can be seen that from Fig. 1 and Fig. 2, and α-Fe are prepared2O3Nano-particle be in ellipsoid, with d-
Ti3C2Tx it is compound and be heat-treated after, d-Ti3C2Tx lamellas are distributed in α-Fe2O3On the surface of nano-particle, and before and after heat treatment
α-Fe2O3Shape apparent variation does not occur, be still ellipsoid.Such a construction increases the electric conductivity of composite material, and
And avoid Ti3C2The accumulation of Tx lamellas, to improve its absorbing property.During heat treatment, cetyl trimethyl bromine
Change ammonium to be carbonized, the carbon of generation is by α-Fe2O3It is reduced to Fe3O4, Fe3O4It is a kind of ferromagnetic substance, thus greatly improved
The magnetism of material is also beneficial to the raising of absorbing property.
Embodiment 2
The present invention provides a kind of preparation methods of magnetism Mxenes polymer composite wave-suction materials, include the following steps：
S1：30mg powdered iron oxide and 300mg cetyl trimethylammonium bromides are added in 400mL deionized waters, and
Ultrasound makes iron oxide be uniformly dispersed in deionized water, and the iron oxide dispersion of cetyl trimethylammonium bromide modification is prepared
Liquid；
S2：The iron oxide dispersion liquid that step S1 is prepared is added dropwise to the Mxenes of a concentration of 0.1mg/mL of 700mL
(Ti3C2Tx) in colloid, for 24 hours, Mxenes (Ti are prepared in magnetic agitation3C2Tx)/ Fe2O3Suspension, then with aperture be 0.22
μm inorganic filter membrane to the Mxenes (Ti that are prepared3C2Tx)/ Fe2O3Suspension is filtered and is done under temperature 60 C
Dry 12h finally obtains Mxenes (Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3Precipitation is placed in tube furnace, in argon atmosphere, with
The heating rate of 4 DEG C/min is heated to 450 DEG C and keeps the temperature 20min, then cooled to room temperature, and black powder is prepared
Mxenes(Ti3C2Tx)/Fe3O4Nanocomposite；
S4：Weigh the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4Nanocomposite 0.1g and Kynoar
0.9g, is added solvent n,N-Dimethylformamide, and ultrasonic 1h makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and poly- inclined
Vinyl fluoride is uniformly mixed, then naturally dry；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold to be placed on hot press, be 210 DEG C in temperature, pressure is to be molded 3h under 15MPa, then pressurize cools down, and is prepared
Mxenes(Ti3C2Tx)/Fe3O4The Kynoar composite wave-suction material of filling.
The iron oxide is α-Fe2O3, it is prepared by the following method to obtain：
Addition 2.73g Iron(III) chloride hexahydrates and 2g urea in 100mL deionized waters, the heating water bath 5h at 90 DEG C, simultaneously
Magnetic agitation is collected by centrifugation the precipitation that reaction generates, and spends ion-cleaning after the reaction was complete, then under the conditions of temperature is 60 DEG C
Dry 12h, is prepared FeOOH, affiliated FeOOH is finally heated to 450 with the heating rate of 5 DEG C/min
DEG C, 2h, then cooled to room temperature are kept the temperature, α-Fe are prepared2O3。
The magnetic Mxenes polymer composite wave-suction material being prepared through this embodiment, in the composite wave-suction material
Mxenes(Ti3C2Tx)/Fe3O4The mass percent of nanocomposite is 10%, Mxenes in the composite wave-suction material
(Ti3C2Tx) it is four layers of few layer or single layer below, Fe3O4For polyhedron, grain size is 200 ~ 300nm.
Embodiment 3
The present invention provides a kind of preparation methods of magnetism Mxenes polymer composite wave-suction materials, include the following steps：
S1：40mg powdered iron oxide and 400mg cetyl trimethylammonium bromides are added in 500mL deionized waters, and
Ultrasound makes iron oxide be uniformly dispersed in deionized water, and the iron oxide dispersion of cetyl trimethylammonium bromide modification is prepared
Liquid；
S2：The iron oxide dispersion liquid that step S1 is prepared is added dropwise to the Mxenes of a concentration of 0.1mg/mL of 600mL
(Ti3C2Tx) in colloid, for 24 hours, Mxenes (Ti are prepared in magnetic agitation3C2Tx)/ Fe2O3Suspension, then with aperture be 0.22
μm inorganic filter membrane to the Mxenes (Ti that are prepared3C2Tx)/ Fe2O3Suspension is filtered and is done under temperature 60 C
Dry 12h finally obtains Mxenes (Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3Precipitation is placed in tube furnace, in argon atmosphere, with
The heating rate of 6 DEG C/min is heated to 450 DEG C and keeps the temperature 40min, then cooled to room temperature, and black powder is prepared
Mxenes(Ti3C2Tx)/Fe3O4Nanocomposite；
S4：Weigh the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4Nanocomposite 0.15g and Kynoar
0.85g, is added solvent n,N-Dimethylformamide, and ultrasonic 1h makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and poly-
Vinylidene is uniformly mixed, then naturally dry；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold to be placed on hot press, be 220 DEG C in temperature, pressure is to be molded 4.5h under 12MPa, then pressurize cools down, and is prepared
Mxenes(Ti3C2Tx)/Fe3O4The Kynoar composite wave-suction material of filling.
The iron oxide is α-Fe2O3, it is prepared by the following method to obtain：
Addition 2.73g Iron(III) chloride hexahydrates and 2g urea in 100mL deionized waters, the heating water bath 5h at 90 DEG C, simultaneously
Magnetic agitation is collected by centrifugation the precipitation that reaction generates, and spends ion-cleaning after the reaction was complete, then under the conditions of temperature is 60 DEG C
Dry 12h, is prepared FeOOH, affiliated FeOOH is finally heated to 450 with the heating rate of 5 DEG C/min
DEG C, 2h, then cooled to room temperature are kept the temperature, α-Fe are prepared2O3。
The magnetic Mxenes polymer composite wave-suction material being prepared through this embodiment, in the composite wave-suction material
Mxenes(Ti3C2Tx)/Fe3O4The mass percent of nanocomposite is 15%, Mxenes in the composite wave-suction material
(Ti3C2Tx) it is four layers of few layer or single layer below, Fe3O4For polyhedron, grain size is 200 ~ 300nm.
Embodiment 4
The present invention provides a kind of preparation methods of magnetism Mxenes polymer composite wave-suction materials, include the following steps：
S1：20mg powdered iron oxide and 300mg cetyl trimethylammonium bromides are added in 300mL deionized waters, and
Ultrasound makes iron oxide be uniformly dispersed in deionized water, and the iron oxide dispersion of cetyl trimethylammonium bromide modification is prepared
Liquid；
S2：The iron oxide dispersion liquid that step S1 is prepared is added dropwise to the Mxenes of a concentration of 0.1mg/mL of 500mL
(Ti3C2Tx) in colloid, for 24 hours, Mxenes (Ti are prepared in magnetic agitation3C2Tx)/ Fe2O3Suspension, then with aperture be 0.22
μm inorganic filter membrane to the Mxenes (Ti that are prepared3C2Tx)/ Fe2O3Suspension is filtered and is done under temperature 60 C
Dry 12h finally obtains Mxenes (Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3Precipitation is placed in tube furnace, in argon atmosphere, with
The heating rate of 5 DEG C/min is heated to 420 DEG C and keeps the temperature 25min, then cooled to room temperature, and black powder is prepared
Mxenes(Ti3C2Tx)/Fe3O4Nanocomposite；
S4：Weigh the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4Nanocomposite 0.2g and Kynoar
0.8g, is added solvent n,N-Dimethylformamide, and ultrasonic 1h makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and poly- inclined
Vinyl fluoride is uniformly mixed, then naturally dry；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold to be placed on hot press, be 225 DEG C in temperature, pressure is to be molded 5.5h under 18MPa, then pressurize cools down, and is prepared
Mxenes(Ti3C2Tx)/Fe3O4The Kynoar composite wave-suction material of filling.
The iron oxide is α-Fe2O3, it is prepared by the following method to obtain：
Addition 2.73g Iron(III) chloride hexahydrates and 2g urea in 100mL deionized waters, the heating water bath 5h at 90 DEG C, simultaneously
Magnetic agitation is collected by centrifugation the precipitation that reaction generates, and spends ion-cleaning after the reaction was complete, then under the conditions of temperature is 60 DEG C
Dry 12h, is prepared FeOOH, affiliated FeOOH is finally heated to 450 with the heating rate of 5 DEG C/min
DEG C, 2h, then cooled to room temperature are kept the temperature, α-Fe are prepared2O3。
The magnetic Mxenes polymer composite wave-suction material being prepared through this embodiment, in the composite wave-suction material
Mxenes(Ti3C2Tx)/Fe3O4The mass percent of nanocomposite is 20%, Mxenes in the composite wave-suction material
(Ti3C2Tx) it is four layers of few layer or single layer below, Fe3O4For polyhedron, grain size is 200 ~ 300nm.
Embodiment 5
The present invention provides a kind of preparation methods of magnetism Mxenes polymer composite wave-suction materials, include the following steps：
S1：10mg powdered iron oxide and 200mg cetyl trimethylammonium bromides are added in 200mL deionized waters, and
Ultrasound makes iron oxide be uniformly dispersed in deionized water, and the iron oxide dispersion of cetyl trimethylammonium bromide modification is prepared
Liquid；
S2：The iron oxide dispersion liquid that step S1 is prepared is added dropwise to the Mxenes of a concentration of 0.1mg/mL of 300mL
(Ti3C2Tx) in colloid, for 24 hours, Mxenes (Ti are prepared in magnetic agitation3C2Tx)/ Fe2O3Suspension, then with aperture be 0.22
μm inorganic filter membrane to the Mxenes (Ti that are prepared3C2Tx)/ Fe2O3Suspension is filtered and is done under temperature 60 C
Dry 12h finally obtains Mxenes (Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3Precipitation is placed in tube furnace, in argon atmosphere, with
The heating rate of 3 DEG C/min is heated to 380 DEG C and keeps the temperature 25min, then cooled to room temperature, and black powder is prepared
Mxenes(Ti3C2Tx)/Fe3O4Nanocomposite；
S4：Weigh the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4Nanocomposite 0.1g and Kynoar
0.9g, is added solvent n,N-Dimethylformamide, and ultrasonic 1h makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and poly- inclined
Vinyl fluoride is uniformly mixed, then naturally dry；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold to be placed on hot press, be 230 DEG C in temperature, pressure is to be molded 5h under 15MPa, then pressurize cools down, and is prepared
Mxenes(Ti3C2Tx)/Fe3O4The Kynoar composite wave-suction material of filling.
The iron oxide is α-Fe2O3, it is prepared by the following method to obtain：
Addition 2.73g Iron(III) chloride hexahydrates and 2g urea in 100mL deionized waters, the heating water bath 5h at 90 DEG C, simultaneously
Magnetic agitation is collected by centrifugation the precipitation that reaction generates, and spends ion-cleaning after the reaction was complete, then under the conditions of temperature is 60 DEG C
Dry 12h, is prepared FeOOH, affiliated FeOOH is finally heated to 450 with the heating rate of 5 DEG C/min
DEG C, 2h, then cooled to room temperature are kept the temperature, α-Fe are prepared2O3。
The magnetic Mxenes polymer composite wave-suction material being prepared through this embodiment, in the composite wave-suction material
Mxenes(Ti3C2Tx)/Fe3O4The mass percent of nanocomposite is 10%, Mxenes in the composite wave-suction material
(Ti3C2Tx) it is four layers of few layer or single layer below, Fe3O4For polyhedron, grain size is 200 ~ 300nm.
Contrast test
In order to verify the α-Fe that regular oxidation iron is prepared with the present invention2O3To magnetic Mxenes polymer composite wave-suction material
The influence of absorbing property, the present invention are also provided with contrast test, and with reference to embodiment 1 ~ 5, it is constant to control other technological parameters, uses
α-the Fe that regular oxidation iron is prepared instead of the present invention2O3, the magnetic Mxenes polymer composite wave-absorbing material that is finally prepared
Expect the magnetic Mxenes polymer composite wave-suction material being prepared significantly lower than embodiment 1 ~ 5 in terms of absorbing property.
Therefore only several embodiments of the present invention are expressed for above example, the description thereof is more specific and detailed, but can not be
And it is interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that for those of ordinary skill in the art, not
Under the premise of being detached from present inventive concept, various modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials, which is characterized in that include the following steps：
S1：Powdered iron oxide and cetyl trimethylammonium bromide are added in deionized water, and ultrasound makes iron oxide exist
It is uniformly dispersed in deionized water, the iron oxide dispersion liquid of cetyl trimethylammonium bromide modification is prepared；
S2：Mxenes (Ti are added dropwise in the iron oxide dispersion liquid that step S1 is prepared3C2Tx) in colloid, magnetic agitation system
It is standby to obtain Mxenes (Ti3C2Tx)/ Fe2O3Suspension, then filtered with inorganic filter membrane, dried, finally obtain Mxenes
(Ti3C2Tx)/Fe2O3Precipitation；
S3：Mxenes (the Ti that step S2 is prepared3C2Tx)/Fe2O3It is deposited in argon atmosphere and first carries out heating reaction, then
Mxenes (Ti are prepared in cooled to room temperature3C2Tx)/Fe3O4Nanocomposite；
S4：In the Mxenes (Ti that step S3 is prepared3C2Tx)/Fe3O4The mixture of nanocomposite and Kynoar
In, n,N-Dimethylformamide is added, carries out ultrasound, makes Mxenes (Ti3C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride
Alkene is uniformly mixed；
S5：Mxenes (the Ti that will be uniformly mixed in step S43C2Tx)/Fe3O4Nanocomposite and polyvinylidene fluoride material dress
Enter mold and first carry out hot pressing, then pressurize cooling, Mxenes (Ti are prepared3C2Tx)/Fe3O4The Kynoar of filling is compound
Absorbing material.
2. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1, feature exist
In：The iron oxide is α-Fe2O3, the α-Fe2O3It is prepared by the following method to obtain：It is added in 100mL deionized waters
2.73g Iron(III) chloride hexahydrates and 2g urea, the heating water bath 5h at 90 DEG C, while magnetic agitation, centrifugation receipts after the reaction was complete
The precipitation that collection reaction generates, and ion-cleaning is spent, then dry 12h under the conditions of temperature is 60 DEG C, hydroxyl oxidation is prepared
Affiliated FeOOH is finally heated to 450 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 2h, then naturally cool to room by iron
α-Fe are prepared in temperature2O3。
3. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1 or 2, feature
It is：The mass ratio of the iron oxide and the cetyl trimethylammonium bromide is 1:10~1:30.
4. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1 or 2, feature
It is：The solid-to-liquid ratio of the iron oxide and the deionized water is 10:100~200mg/mL.
5. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1 or 2, feature
It is：The iron oxide and the Mxenes (Ti3C2Tx mass ratio) is 15:85~85:85.
6. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1 or 2, feature
It is：Mxenes (the Ti3C2Tx)/Fe3O4The mass percent of composite material and the Kynoar is 5 ~ 20%:80~
95%。
7. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1 or 2, feature
It is：In the step S3, the condition for heating reaction is to be heated to 350 ~ 500 DEG C with the heating rate of 3 ~ 7 DEG C/min, heat preservation
15~45min。
8. a kind of preparation method of magnetism Mxenes polymer composite wave-suction materials according to claim 1 or 2, feature
It is：In the step S4, the temperature of hot pressing is 200 ~ 240 DEG C, and pressure is 10 ~ 20MPa, and the time is 2 ~ 6h.
9. a kind of magnetism Mxenes polymer composite wave-suction materials, it is characterised in that：The composite wave-suction material is wanted according to right
The method described in any one of 1 ~ 8 claim is asked to be prepared, Mxenes (Ti in the composite wave-suction material3C2Tx)/
Fe3O4The mass percent of nanocomposite is 5% ~ 20%, the Mxenes (Ti3C2Tx)/Fe3O4In nanocomposite
Fe3O4Mass percent be 14.6% ~ 49.8%.
10. a kind of magnetism Mxenes polymer composite wave-suction materials according to claim 9, it is characterised in that：It is described multiple
Close Mxenes (Ti in absorbing material3C2Tx) it is four layers of few layer or single layer below, the Fe3O4For polyhedron, grain size is
200~300nm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810249523.8A CN108342036B (en) | 2018-03-26 | 2018-03-26 | Magnetic Mxenes polymer composite wave-absorbing material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810249523.8A CN108342036B (en) | 2018-03-26 | 2018-03-26 | Magnetic Mxenes polymer composite wave-absorbing material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108342036A true CN108342036A (en) | 2018-07-31 |
| CN108342036B CN108342036B (en) | 2020-05-15 |
Family
ID=62958232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810249523.8A Active CN108342036B (en) | 2018-03-26 | 2018-03-26 | Magnetic Mxenes polymer composite wave-absorbing material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108342036B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN111978694A (en) * | 2020-08-14 | 2020-11-24 | 华南理工大学 | Polylactic acid composite material with tensile resistance and impact resistance and preparation method thereof |
| CN112047386A (en) * | 2020-08-27 | 2020-12-08 | 西北工业大学 | Heating modified MXene/ferroferric oxide composite wave-absorbing material and preparation method thereof |
| CN113336986A (en) * | 2021-06-03 | 2021-09-03 | 陕西科技大学 | Preparation method of oriented gamma-phase PVDF/CTAB composite film |
| FR3118774A1 (en) * | 2021-01-12 | 2022-07-15 | Arkema France | THERMOPLASTIC COMPOSITE MATERIAL FOR COMPOSITE TUBULAR STRUCTURES |
| CN115245498A (en) * | 2021-12-28 | 2022-10-28 | 温州医科大学 | Method for preparing near infrared absorption magnetic nano particles |
| CN116769326B (en) * | 2023-05-30 | 2024-03-29 | 南昌大学 | MXene-based wave-absorbing material, preparation method and application |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951916A (en) * | 2014-04-29 | 2014-07-30 | 南昌航空大学 | RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof |
| CN105470486A (en) * | 2015-12-25 | 2016-04-06 | 陕西科技大学 | Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material |
| EP3187908A1 (en) * | 2014-08-29 | 2017-07-05 | National Institute for Materials Science | Electromagnetic wave absorbing/radiating material, method for manufacturing same, and infrared source |
| CN107099054A (en) * | 2017-05-12 | 2017-08-29 | 深圳大学 | Ti3C2The preparation method of MXene/ polymer composite wave-suction materials |
| CN107603087A (en) * | 2017-10-19 | 2018-01-19 | 渭南高新区火炬科技发展有限责任公司 | Composite wave-absorbing material and preparation method thereof |
| CN107694510A (en) * | 2017-11-14 | 2018-02-16 | 南昌大学 | A kind of two-dimensional magnetic MXene is to dyeing waste water Methylene Blue minimizing technology |
-
2018
- 2018-03-26 CN CN201810249523.8A patent/CN108342036B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951916A (en) * | 2014-04-29 | 2014-07-30 | 南昌航空大学 | RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof |
| EP3187908A1 (en) * | 2014-08-29 | 2017-07-05 | National Institute for Materials Science | Electromagnetic wave absorbing/radiating material, method for manufacturing same, and infrared source |
| CN105470486A (en) * | 2015-12-25 | 2016-04-06 | 陕西科技大学 | Preparation method of granular tin dioxide/two-dimensional nano titanium carbide composite material |
| CN107099054A (en) * | 2017-05-12 | 2017-08-29 | 深圳大学 | Ti3C2The preparation method of MXene/ polymer composite wave-suction materials |
| CN107603087A (en) * | 2017-10-19 | 2018-01-19 | 渭南高新区火炬科技发展有限责任公司 | Composite wave-absorbing material and preparation method thereof |
| CN107694510A (en) * | 2017-11-14 | 2018-02-16 | 南昌大学 | A kind of two-dimensional magnetic MXene is to dyeing waste water Methylene Blue minimizing technology |
Non-Patent Citations (3)
| Title |
|---|
| REN ZOU，ET AL.: "Self-assembled MXene(Ti3C2Tx)/a-Fe2O3 nanocomposite as negative electrode material for supercapacitors", 《ELECTROCHIMICA ACTA》 * |
| YUCHANG QING，ET AL.: "Titanium carbide(MXene) nanosheets as promising microwave absorbers", 《CERAMICS INTERNATIONAL》 * |
| 杜军 等: "纳米Fe3O4/PVDF磁性复合膜的原位制备及表征", 《物理化学学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591641A (en) * | 2019-01-25 | 2019-12-20 | 陕西科技大学 | Fe2O3@ MXene composite powder and preparation method thereof |
| CN111978694A (en) * | 2020-08-14 | 2020-11-24 | 华南理工大学 | Polylactic acid composite material with tensile resistance and impact resistance and preparation method thereof |
| CN111978694B (en) * | 2020-08-14 | 2021-06-08 | 华南理工大学 | Polylactic acid composite material with tensile resistance and impact resistance and preparation method thereof |
| CN112047386A (en) * | 2020-08-27 | 2020-12-08 | 西北工业大学 | Heating modified MXene/ferroferric oxide composite wave-absorbing material and preparation method thereof |
| FR3118774A1 (en) * | 2021-01-12 | 2022-07-15 | Arkema France | THERMOPLASTIC COMPOSITE MATERIAL FOR COMPOSITE TUBULAR STRUCTURES |
| WO2022152995A1 (en) * | 2021-01-12 | 2022-07-21 | Arkema France | Composite thermoplastic material for composite tubular structures |
| CN113336986A (en) * | 2021-06-03 | 2021-09-03 | 陕西科技大学 | Preparation method of oriented gamma-phase PVDF/CTAB composite film |
| CN115245498A (en) * | 2021-12-28 | 2022-10-28 | 温州医科大学 | Method for preparing near infrared absorption magnetic nano particles |
| CN116769326B (en) * | 2023-05-30 | 2024-03-29 | 南昌大学 | MXene-based wave-absorbing material, preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108342036B (en) | 2020-05-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108342036A (en) | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof | |
| Zhang et al. | Thermal conversion of an Fe 3 O 4@ metal–organic framework: a new method for an efficient Fe–Co/nanoporous carbon microwave absorbing material | |
| CN106753237B (en) | A kind of graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof | |
| CN108834389A (en) | A kind of preparation method of the derivative nano combined absorbing material of porous carbon/multi-walled carbon nanotube of bimetallic organic frame | |
| CN107949266B (en) | A kind of three-dimensional porous flower-like structure cobalt/carbon nano composite electromagnetic wave absorption material and preparation method thereof | |
| CN107033842B (en) | A kind of composite wave-absorbing agent, preparation method and applications | |
| CN107293700A (en) | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and battery | |
| CN109664566A (en) | A kind of lightweight broad-band band multi-layer structured wave absorbing composite material and preparation method thereof | |
| CN102533216A (en) | Ferroferric oxide/reduced graphene oxide composite wave-absorbing material with hollow hemisphere structure and preparation method | |
| CN110283570A (en) | A kind of FeCo@MXene core-shell structure composite wave-suction material and preparation method thereof | |
| Peng et al. | Synthesis and microwave absorption properties of Fe 3 O 4@ BaTiO 3/reduced graphene oxide nanocomposites | |
| CN108047806B (en) | graphene/Ag-carbon microsphere aerogel coating and preparation method and application thereof | |
| CN107938432A (en) | A kind of preparation method of carbon nanometer paper composites | |
| CN113462357A (en) | Wave-absorbing particles and preparation method and application of composite material thereof | |
| CN104883868B (en) | A kind of preparation method being electromagnetically shielded with magnetic material/graphene paper | |
| CN108154947A (en) | A kind of composite material of graphene coated resin particle and its preparation method and application | |
| CN111019603A (en) | Cobaltosic oxide/carbon fiber composite material and preparation method and application thereof | |
| CN114073919B (en) | Carbon-magnetic metal dispersion type hollow composite microsphere and preparation method and application thereof | |
| CN114920232A (en) | C/Mo with porous core-shell heterostructure 2 C@SnS 2 Wave-absorbing material and preparation method thereof | |
| CN111420619B (en) | Preparation method of cellulose-chitosan/PANI composite aerogel | |
| CN110423516B (en) | Ink, preparation method thereof and gas sensor film | |
| CN114520419A (en) | Preparation method of cobalt-based metal organic framework derivative wave absorbing agent with nano composite structure | |
| CN110305429A (en) | A kind of flexibility absorbing material and preparation method thereof | |
| CN109705677B (en) | Electrothermal coating based on graphene three-dimensional network structure carbon coating technology and preparation method thereof | |
| CN115843172A (en) | Hollow carbon-loaded metal nickel particle, preparation method and application of microwave absorption |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |